Hazardous Waste Combustion Unit · American Society for Testing and Materials (ASTM). “Annual Book of ASTM Standards.” Philadelphia, Pennsylvania. Annual Series. U.S. Environmental

Tetra Tech EM Inc.

Hazardous Waste Combustion UnitPermitting Manual

How To Conduct A Laboratory Audit

COMPONENT 5

UNITED STATES

EN

VIRO

NM

ENTALPROTECTIO

NA

GEN

CY

U.S. EPA Region 6 Center for CombustionScience and Engineering

6 752 31 4

COMPONENT FIVE

HOW TO CONDUCT A LABORATORY AUDIT

JANUARY 1998

COMPONENT 5—HOW TO CONDUCT A LABORATORY AUDIT

U.S. EPA Region 6Center for Combustion Science and Engineering i

CONTENTS

Section Page

ABBREVIATIONS AND ACRONYMS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ivBIBLIOGRAPHY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . v

1.0 INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-12.0 PREAUDIT ACTIVITIES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3

2.1 OBTAINING BASIC LABORATORY INFORMATION . . . . . . . . . . . . . . . . . . . 5-4

2.1.1 Gathering Information Regarding Laboratory Name, Address, and TelephoneNumbers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6

2.1.2 Gathering Contact Personnel Information . . . . . . . . . . . . . . . . . . . . . . . . . . 5-72.1.3 Reviewing the Relationship of a Laboratory to the Facility . . . . . . . . . . . . . 5-82.1.4 Reviewing the Matrixes to be Analyzed and the Analytical Methods . . . . 5-10

2.2 GATHERING INFORMATION FROM THE FACILITY TRIAL BURN PLAN ANDQUALITY ASSURANCE PROJECT PLAN . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11

2.2.1 Organization of Personnel, Responsibilities, and Qualifications . . . . . . . . 5-132.2.2 Quality Assurance Objectives . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-142.2.3 Sample Monitoring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-172.2.4 Sample Handling, Traceability, and Holding Times . . . . . . . . . . . . . . . . . 5-192.2.5 Calibration Procedures and Frequency . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-202.2.6 Analytical Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-222.2.7 Internal Quality Control Checks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-242.2.8 Data Reduction, Data Validation, and Data Reporting . . . . . . . . . . . . . . . 5-252.2.9 Assessment Procedures for Accuracy and Precision . . . . . . . . . . . . . . . . . 5-262.2.10 Audit Procedures, Corrective Action, and QA Reporting . . . . . . . . . . . . . 5-27

2.3 SCHEDULING THE AUDIT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-292.4 ASSEMBLING THE AUDIT TEAM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-312.5 PREPARING A LABORATORY-SPECIFIC CHECKLIST . . . . . . . . . . . . . . . . . 5-33

3.0 CONDUCTING THE AUDIT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-35

3.1 CONDUCTING THE PREAUDIT BRIEFING . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-36

3.1.1 Introducing Key Personnel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-373.1.2 Stating the Purpose of the Audit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-383.1.3 Describing the Scope of the Audit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-493.1.4 Answering Questions and Addressing Issues From Laboratory Personnel 5-41

CONTENTS (Continued)

Section Page


U.S. EPA Region 6Center for Combustion Science and Engineering ii

3.2 CONDUCTING THE WALKTHROUGH . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-42

3.2.1 Sample Receiving, Storage, and Custody Area . . . . . . . . . . . . . . . . . . . . . 5-443.2.2 Organic Sample Preparation Laboratory . . . . . . . . . . . . . . . . . . . . . . . . . . 5-473.2.3 Organic Analytical Laboratory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-493.2.4 Inorganic Sample Preparation Laboratory . . . . . . . . . . . . . . . . . . . . . . . . . 5-533.2.5 Inorganic Analytical Laboratory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-563.2.6 Physical Parameter Laboratory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-603.2.7 Data Reduction and Reporting Procedures . . . . . . . . . . . . . . . . . . . . . . . . 5-643.2.8 Archival and Disposal of Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-66

3.3 COMPLETING THE AUDIT CHECKLIST . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-68

3.3.1 Answering the Checklist Questions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-693.3.2 Noting Omissions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-713.3.3 Noting Deficiencies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-723.3.4 Noting Additional Questions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-74

3.4 CONDUCTING THE AUDIT DEBRIEFING . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-75

4.0 POST AUDIT ACTIVITIES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-77

4.1 REVIEWING AUDIT INFORMATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-784.2 ANALYSIS OF DEFICIENCIES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-80

4.2.1 Comparing Findings Between Audit Team Members . . . . . . . . . . . . . . . . 5-824.2.2 Identifying Major Concerns . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-844.2.3 Identifying Minor Concerns . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-864.2.4 Preparing Preliminary Comments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-88

4.3 PREPARING THE AUDIT REPORT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-90

4.3.1 Overview of the Trial Burn Test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-914.3.2 Overview of the Laboratory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-924.3.3 Summarizing Concerns . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-944.3.4 Summarizing Comments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-964.3.5 Preparing Recommendations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-974.3.6 Preparing the Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-98


U.S. EPA Region 6Center for Combustion Science and Engineering iii

EXHIBITS

Exhibit Page

2.2.2-1 EXAMPLE SUMMARY TABLE OF PRECISION AND ACCURACY OBJECTIVES . . . . 15

ATTACHMENTS

Attachment

A LABORATORY AUDIT CHECKLIST


U.S. EPA Region 6Center for Combustion Science and Engineering iv

ABBREVIATIONS AND ACRONYMS

CERI Center for Environmental Research InformationGC/MS Gas chromatography/mass spectrometryICP Inductively coupled plasmaOSWER Office of Solid Waste and Emergency ResponsePM Particulate matterPOHC Principal organic hazardous constituentQAPP Quality assurance project planQA/QC Quality assurance/quality controlRCRA Resource Conservation and Recovery ActSOP Standard operating procedureSVOC Semivolatile organic compoundTBP Trial burn planU.S. EPA U.S. Environmental Protection AgencyVOC Volatile organic compoundVOST Volatile organic sampling train


U.S. EPA Region 6Center for Combustion Science and Engineering v

BIBLIOGRAPHY

American Society for Testing and Materials (ASTM). “Annual Book of ASTM Standards.” Philadelphia, Pennsylvania. Annual Series.

U.S. Environmental Protection Agency (EPA). 1988. “Resource Conservation and Recovery Act(RCRA) Laboratory Audit Procedures (RCRA Ground-Water Monitoring Systems).” Officeof Solid Waste and Emergency Response (OSWER) 9950.4. RCRA Enforcement Division. Washington, D.C. September.

U.S. EPA. 1989. “Handbook: Hazardous Waste Incineration Measurement Guidance Manual.” Volume III of the Hazardous Waste Incineration Guidance Series. OSWER. Washington,D.C. EPA/625/6-89/021. June.

U.S. EPA. 1990. “Handbook: Quality Assurance/Quality Control (QA/QC) Procedures forHazardous Waste Incineration.” Center for Environmental Research Information (CERI). Cincinnati, Ohio. EPA/625/6-89/023. January.

U.S. EPA. 1996. “Test Methods for Evaluating Solid Wastes: Physical/Chemical Methods. Update III (SW-846).” OSWER. Washington, D.C. December.

U.S. EPA. 1997. “Generic Quality Assurance Project Plan (QAPP).” Center for CombustionScience and Engineering, Multimedia Planning and Permitting Division, U.S. EPA Region 6. Dallas, Texas. December.

U.S. EPA. 1997. “Generic Trial Burn Plan (TBP).” Center for Combustion Science and Engineering,Multimedia Planning and Permitting Division, U.S. EPA Region 6. Dallas, Texas. December.


U.S. EPA Region 6Center for Combustion Science and Engineering 5-1

1.0 INTRODUCTION

Regulations: No regulations are applicable to this section of the manual.

Guidance: No specific references are applicable to this section of the manual.

Explanation: Laboratory systems must be audited to ensure that the highest quality results forboth stack gases and waste feed samples are produced. Laboratory auditfindings determine the degree of confidence the permit writer has in theanalytical results reported by the facility. The analytical results are needed tosupport permit conditions and the risk assessment. Because facilities maycontract more than one laboratory for analyses, it may be necessary to audit eachlaboratory associated with the trial burn.

The laboratory audit consists of (1) observing sample receipt, storage,preparation, and analysis, data review, and trial burn sample reporting;(2) evaluating raw data generated by the laboratory; and (3) reviewing projectrecords. Laboratory audit activities are categorized into three groups: (1) pre-audit activities (Section 2.0), (2) audit activities (Section 3.0), and (3) post-auditactivities (Section 4.0). The following sections will address each activitycategory, with detailed descriptions. In addition, general laboratory safety andsample or waste disposal practices should be reviewed.

Attachment A is an example of a checklist that can be used to assist in thelaboratory audit. This review checklist can be used to ensure that all activitiesassociated with a laboratory audit are completed.

Check For: Each auditor should review the following sections to ensure they are prepared forthe following activities:

“ Pre-audit Activities (Section 2.0)

“ Conducting the Audit (Section 3.0)

“ Post-Audit Activities (Section 4.0)

Example Situation: Lois and Clark of Metropolis have been selected to conduct laboratory audits inconnection with the permitting process for several facilities. In the case of onefacility, Clark needs to audit a laboratory for a trial burn, but he does not have thecompleted trial burn quality assurance project plan (QAPP).



Example Action: To complete the audit successfully, Clark needs to have copies of the trial burnQAPP, trial burn plan (TBP), and access to personnel. Clark asks that thefacility provide him with copies of the trial burn QAPP and TBP, and he asks thelaboratory to allow him access to laboratory personnel.



Notes:



2.0 PRE-AUDIT ACTIVITIES



Explanation: Several major steps must be accomplished to organize and conduct a laboratoryaudit. Each of the major steps is described in the following sections.

Check For: The following tasks should be completed by the permit writer preparing for theaudit:

“ Obtain basic laboratory information (see Section 2.1).

“ Review facility TBP and trial burn QAPP (see Section 2.2).

“ Schedule the audit with the laboratory (see Section 2.3).

“ Assemble the audit team (see Section 2.4).

“ Prepare a laboratory-specific audit checklist (see Section 2.5).

Example Situation: Training a new permit writer or staff member for a laboratory audit can bechallenging even for staff who have chemistry training. Pre-audit activities arecritical to the success of an audit. Basic laboratory information, such as whichlaboratories are being used for analysis, may not be clear from TBP or trial burnQAPP information, and the audit team may have to obtain this information fromthe testing firm or trial burn facility manager.

Example Comments: A successful audit will occur when it is organized in a thorough, step-by-stepfashion similar to the guidance provided in this document. Conducting alaboratory audit without thorough planning will usually result in an incompleteaudit.

Notes:



2.1 OBTAINING BASIC LABORATORY INFORMATION



Explanation: Basic laboratory information should be made available to the permit writer by thefacility. Multiple laboratories may be contracted by a facility to analyze trial burnsamples. It is important to obtain information from all laboratories and tounderstand the relationships among the facility, contractor laboratories, andsubcontractor laboratories. This information is useful for verifying the accuratetransfer of project-specific analysis requests and QC information from the facilityto all contractors and subcontractors. Frequently, the facility contracts with anorganization to prepare the TBP and trial burn QAPP, and may hire sampling andanalytical contractors. It is essential to understand (1) the testing programorganization, (2) the contracting responsibilities of the various parties, (3) who isresponsible for communicating key information to the laboratories, and (4) who isthe resource for the laboratory regarding questions about samples or analyses.

Check For: The following information should be obtained for each contracted laboratory:

“ Laboratory name, address, and telephone, facsimile, and e-mail numbers(Section 2.1.1)

“ Names and titles of contact personnel (Section 2.1.2)

“ Relationship of laboratory to facility, sampling organization, ororganization preparing the TBP and trial burn QAPP (Section 2.1.3)

“ Matrices to be analyzed, methods of analysis for each, number ofsamples, and delivery schedule of sample to the laboratory (Section2.1.4)

Each of the items may be summarized in tabular format, as presented in thefollowing example situation. Each of the listed items is discussed in the followingsubsections.

Example Situation: In preparation for conducting a laboratory audit, Lois receives the followinginformation from the facility.

Laboratory A has been advised by the regular contact at Facility X that it will beanalyzing waste feed samples from a trial burn. The samples should arrive withinthe next 2 to 3 weeks, and the chain-of-custody documentation will provide all ofthe information that the laboratory needs for the analyses.



Name andAddress Contacts Relationship Matrix Analysis Method

Laboratory A Lab Director Subcontractor to Waste feed Viscosity SW-8461111 1st Street Mr. John Doe Facility X’s BIF metals 6010AAnywhere, (555) 555-5551 environmental Chloride 9250USA QA Officer consultant1-800-555-5555 Ms. Jane Smith

(555) 555-5552

Laboratory B Lab Director Subcontractor to Stack gas Volatiles SW-8462222 1st Street Mr. John Doe Facility X’s Semivolatiles 8260Anywhere, (555) 555-5551 environmental 8270USA QA Officer consultant1-800-555-5555 Ms. Jane Smith

(555) 555-5552

Laboratory C Lab Director Subcontractor to Stack gas Dioxins and SW-8463333 1st Street Mr. John Doe Laboratory B furan 8290Anywhere, (555) 555-5551USA QA Officer 1-800-555-5555 Ms. Jane Smith

(555) 555-5552

Example Action: Lois determines that the amount of information provided for Laboratory A isunacceptable. Lois advises both the facility and the laboratory that Laboratory Ashould take no action other than logging in samples, as received, and ensuringappropriate ambient or subambient storage, until (1) the appropriate technicalcontact (who can respond to technical questions regarding trial burn samples) hasbeen established, and (2) the laboratory has received a copy of the trial burnQAPP. If the laboratory cannot receive a complete copy of the trial burnQAPP, Lois requests that the facility provide tables specifying required analyses,QC measures, and control limits to the laboratory.

Notes:



2.1.1 Gathering Information Regarding Laboratory Name, Address, and Telephone Numbers



Explanation: The laboratory name, address, telephone, and facsimile numbers are basicinformation needed to (1) distinguish the laboratories, (2) direct correspondence,and (3) locate the laboratory for the audit. This information should be providedby the facility and located in the trial burn QAPP.

Check For: “ Whether the laboratory name is the most recent

“ Whether the laboratory address is accurate so that it could be used inphysically locating the facility (for example, whether the address is apost office box or a street numbers)

“ Whether the telephone and facsimile numbers for the main switchboardand any key personnel contacted are correct

Example Situation: In reviewing laboratory information supplied by the facility, Clark suspects that the laboratory name and address have recently changed because it is referencedby different names in the documents reviewed. Confusion may increase if thelaboratory is part of a network of laboratories.

Example Action: Clark asks that the facility clarify the basic laboratory information before he begins any other pre-audit activities.

Notes:



2.1.2 Gathering Contact Personnel Information



Explanation: The key contact for the laboratory may be any one of the following persons. It isimportant to obtain the name and title of the person responsible for overall project management. Accurate information can ensure that the appropriate decision-maker is notified of project requirements.

• Company president• Laboratory director or manager• Quality assurance (QA) officer or manager• Project manager or scientist• Operations manager• Laboratory supervisor• Client services coordinator

Check For: “ Whether the name of the key contact is accurate

“ Whether the telephone and facsimile numbers obtained in the basiclaboratory information can be used to reach the key contact

“ Whether the key contact has appropriate authority to halt laboratorywork when QC is jeopardized

“ Whether the key person has appropriate authority to implement projectrequirements within the laboratory

Example Situation: Clark reviews the project organization in the trial burn QAPP, which identifiesthe QA manager as the key contact. However, Clark remembers that althoughlaboratories often consider the QA manager to be the key contact, they may nothave the authority to implement project requirements. After reviewinginformation from the facility further, Clark determines that the informationprovided is inadequate to determine the chain-of-command at the laboratory, andthat he cannot proceed with the audit.

Example Action: Clark asks that the facility provide the names of key laboratory personnel and asummary of their job responsibilities so that he knows who should be contactedfor the audit.

Notes:



2.1.3 Reviewing the Relationship of a Laboratory to the Facility



Explanation: Understanding the relationship of the laboratory to the facility is importantbecause it determines how project requirements are transferred to the laboratory. Often, the laboratory is a subcontractor to an environmental firm contracteddirectly by the facility. If there is more than one intermediary between thefacility and the laboratory, vital project-specific requirements may not betransferred effectively, which may result in poor data quality or unusable data. The project organization should be presented as shown in Section 4 of the U.S.EPA Region 6 generic trial burn QAPP, including names of specific individualsand details of all individual organizations.

Check For: “ Whether the laboratory is directly contracted by the facility

“ Whether the laboratory is contracted by a facility environmentalcontractor

“ Whether the laboratory is a subcontractor to a primary environmentalcontractor laboratory

“ Whether the relationship is understood by the laboratory

“ Whether the laboratory knows the name of the person and organizationto whom it directly reports

Example Situation: If the laboratory is a subcontractor to an environmental firm contracted by thefacility for the trial burn, key project-specific requirements may not betransferred effectively to the laboratory. If the TBP or trial burn QAPP havenever been transferred data generated from uninformed laboratories may notmeet data quality objectives established in the trial burn QAPP. For example,reporting limits required by the trial burn QAPP to meet permit requirements formetals emissions may not be achieved thereby compromising data usability.

If the analytical laboratory is working directly for the facility on similar samplematrices for a different project, ensure that trial burn analysis requirements aremet. In one recent case, a laboratory was analyzing gross water content for aclient; this analysis consumed the entire sample sent from the facility. Whileconducting an audit at this same time, Lois verified that the appropriate laboratorycontact had received the facility’s TBP and trial burn QAPP, which required atotal waste analysis. Had the analytical laboratory proceeded in its normalfashion, without first reviewing the facility documentation, all of the waste fuel



samples would have been consumed, and water content results critical to the finaldata would not have been detailed enough to meet trial burn requirements.

Example Action: The auditor must understand the relationship between the laboratory and thefacility and verify that trial burn QAPP and TBP requirements have beenforwarded to the laboratory.

Notes:



2.1.4 Reviewing the Matrices to be Analyzed and the Analytical Methods



Explanation: Before the audit is conducted, the auditor should determine which matrices willbe received by the laboratory and select the analyses. One matrix may beanalyzed by different laboratories. This information may be obtained eitherdirectly from the facility or from the trial burn QAPP; guidance is provided inAppendix A of the U.S. EPA 1990 QA/QC Handbook. This information isnecessary for preparing laboratory-specific audit checklists.

Check For: “ Whether Section 9.0 of the U.S. EPA Region 6 generic trial burn QAPPprovides consistent information regarding matrices, analyses, methods,QC criteria, and laboratories

“ Whether the laboratory knows in advance which matrices will beanalyzed, the types of analysis, and the methods to be used

“ Whether the laboratory has experience in analyzing the matricesindicated in the trial burn QAPP and TBP

Example Situation: In reviewing the trial burn QAPP provided by the facility for the laboratory audit,Clark discovers that the document specifies test methods that are inconsistentwith the listed matrices: particulate matter (PM) analysis on waste feed samplesand viscosity analysis on stack gas samples. These methods are clearlyinaccurate when compared to method requirements in Chapters 5, 7, and 8 of theU.S. EPA 1990 QA/QC Handbook.

Example Action: If the laboratory has received the trial burn QAPP in advance of sample receipt,the key laboratory staff member (possibly the laboratory director or the QAmanager) should review the trial burn QAPP and call the key contact at thefacility (or at the contractor) and obtain the correct matrix-specific test method. If this process has not occurred prior to the audit, the auditors should call thefacility key contact to confirm the correct test method (as Clark does in thiscase). If the laboratory has not received a copy of the updated trial burn QAPPand is relying on outdated incorrect information from chain-of-custodydocumentation, the laboratory may not be aware of the error.

Notes:



2.2 GATHERING INFORMATION FROM THE FACILITY TRIAL BURN PLAN ANDQUALITY ASSURANCE PROJECT PLAN

Regulations: Not applicable to this section of the manual.


Explanation: A detailed discussion on reviewing the facility TBP and trial burn QAPP ispresented in Components 1 and 2 of this manual. This section will discuss keyitems in the TBP and trial burn QAPP that the auditor needs to extract to auditthe laboratory. The trial burn QAPP contains information that is most relevant tothe laboratory. The information necessary for the laboratory audit is discussed indetail in subsequent sections of this component. Specific information from thetrial burn QAPP should be checked against guidance documents, and used toformulate the laboratory-specific checklist. The auditor should briefly note duringthis activity whether all relevant sections of the U.S. EPA 1990 QA/QCHandbook are addressed in the trial burn QAPP.

Check For: The following information that must be gathered from the TBP and trial burnQAPP is discussed in the following subsections:

“ Organization of personnel, responsibilities, and qualifications (see Section 2.2.1)

“ QA/QC objectives (see Section 2.2.2)

“ Sampling and monitoring procedures (see Section 2.2.3)

“ Sample handling, traceability, and holding times (see Section 2.2.4)

“ Specific calibration procedures and frequency (see Section 2.2.5)

“ Analytical procedures (see Section 2.2.6)

“ Specific internal QC checks (see Section 2.2.7)

“ Data reduction, validation, and reporting (see Section 2.2.8)

“ Assessment procedures for accuracy, precision, and completeness (see Section 2.2.9)

“ Audit procedures, corrective action, and QA reporting (see Section2.2.10)

The auditor should also check to ensure the following:



“ Whether correct sampling and analytical methods are specified

“ Whether any exceptions to the analytical procedures described in themethods are noted and justified

Example Situation: During a laboratory audit, Lois meets with the QA/QC manager to discuss adiscrepancy between the analytical procedures normally used by the laboratoryfor the facility and those described in the trial burn QAPP. The trial burn QAPPprovides minimal discussion of analytical procedures, simply specifying that“analytical methods are routine and do not require further discussion.” However,based on prior experience with waste feed samples from the facility, thelaboratory knows that waste feed samples are usually composited andhomogenized prior to any analysis. Compositing and ensuring homogeneity arenot routine procedures for the analytical methods. These procedures should beclearly described in the trial burn QAPP. If compositing is not completedcorrectly, the resulting sample will not be representative.

Example Action: Lois advises the laboratory not to prepare or analyze the samples until thediscrepancy between the trial burn QAPP and prior laboratory instructions isresolved. If the trial burn QAPP is reviewed before samples are submitted to thelaboratory, the auditor should point out the deficiency in the trial burn QAPP tothe author so that the correct information can be added (as Lois does in thiscase). If the trial burn QAPP cannot be revised prior to testing, a memorandumdescribing the revision to the analytical method should be prepared by the facilityor the contractor and supplied to the laboratory so that the laboratory is aware ofthe correct, modified procedures to be followed before samples prepared andanalyzed.

Notes:



2.2.1 Organization of Personnel, Responsibilities, and Qualifications



Explanation: Section 4.0 of the U.S. EPA Region 6 generic trial burn QAPP presents (1)overall project management, (2) relationships of laboratories to the facility, and(3) lines of authority. Often, the project organizational chart will specify thenames and responsibilities of key laboratory personnel. If this information is notprovided in the trial burn QAPP (for example, when sampling and analyticalcontractors have not been selected at the time of trial burn QAPP approval), thisinformation should be obtained from the key contact at the facility or thecontractor who is coordinating sampling and analytical activities.

Check For : “ Relationships between laboratories and facility

“ Lines of authority (which also represent lines of information transfer)

“ Names and responsibilities of key laboratory personnel

Example Situation: In preparing for a laboratory audit, Clark notes that the trial burn QAPP indicatesthat the laboratory manager also serves as the laboratory QA officer. The trialburn QAPP also indicates that the laboratory is subcontracted by the facility’scontractor environmental firm. This information enables Clark to correctlyidentify who is responsible for laboratory quality and how project requirementsare transferred to the laboratory.

Example Comments: The auditor must be assured that the laboratory manager can be objective inimplementing of the QC program. For example, the laboratory manager cannotlet operating expenses influence the determination to conduct certain QCprocedures.

Notes:



2.2.2 Quality Assurance Objectives



Explanation: Section 5 of the U.S. EPA Region 6 generic trial burn QAPP states specificprecision, accuracy, and completeness objectives for each analysis. Theseparameters are typically consistent with, or more stringent than, the requirementsestablished in Section 2.1.5 and Table 2-3 of the U.S. EPA 1990 QA/QCHandbook. It is important to review the QA objectives in the approved QAPPbefore conducting the laboratory audit.

Check For: “ Whether the audit checklist contains project-specific trial burn QAPPcriteria for accuracy and precision (this may be necessary, becauseproject-specific criteria may be different from the criteria stated in theguidance document)

Example Situation: In reviewing the approved QAPP, Clark notes that the trial burn QAPP (seeExhibit 2.2.2-1, page 5-15) states that the accuracy criterion for the matrix spikeof 1,2,3-trichlorobenzene (a principal organic hazardous constituent [POHC]) is50 to 130 percent recovery. However, the laboratory’s working QAPP statesthat the accuracy criterion is 40 to 160 percent recovery. The laboratory QAPPindicates a recovery range that is less stringent than stated in the laboratory’strial burn QAPP.

Example Action: Clark asks that the laboratory change the criterion to agree with the approvedtrial burn QAPP.

Notes:



EXHIBIT 2.2.2-1

EXAMPLE SUMMARY TABLE OF PRECISION AND ACCURACY OBJECTIVES

Parameter Matrix QC Procedure Precision

AccuracyMean

Recovery%

Semivolatile Waste Feed Isotopically labeled POHC* <35% RSD 50 - 130%POHC (solid or liquid spiked as a surrogate into recovery(1,2,3-trichloro- organic waste) every samplebenzene) Ash

Matrix spike with POHC; N/A 50 - 130%one sample per matrix recovery

1 duplicate sample analysis <35% RSD N/Aper matrix

Stack emissions Isotopically labeled POHC* <40 RPD 50 - 150%spiked as surrogates into (<35 RSD recoveryeach component of the if moreSVOST than 2)

Matrix spike with POHC; N/A 50 - 150%one sample train (each recoverycomponent) per trial burn

1 duplicate sample analysis of <50 RPD N/Aall components of 1 sampletrain with highest POHClevel

Particulate Stack emission Balance calibration with 500 N/A (499.5 - 500.4)mg weight (± 0.5 mg)

Chlorine Aqueous waste Duplicate analysis for 1 run 20 N/ASludge 20 N/ASolid wastes 20 N/AOrganic liquid 20 N/AwastesBlind unknowns 100 ± 10

Hydrogen NaOH Chloride standard in water N/A 100 ± 15Chloride solution/water

NaOH 30 N/Asolution/water

Duplicate analysis for 1 run





EXHIBIT 2.2.2-1 (Continued)

EXAMPLE SUMMARY TABLE OF PRECISION AND ACCURACY OBJECTIVES

Notes:

mg = MilligramN/A = Not applicablePOHC = Principal organic hazardous constituentRPD = Relative percent differenceRSD = Relative standard deviation*Isotopically labeled POHC = C-hexachlorobenzene13

= C -1,2,4,5-tetrachlorobenzene136



2.2.3 Sample Monitoring



Explanation: Section 6.0 of the U.S. EPA Region 6 generic trial burn QAPP is not intended torepeat the sampling details that are discussed in the TBP, but it should contain atable listing all sampling points, frequency, and total number of samples plus afield QC sample. The auditor can use information from this section to preparethe audit checklist with regard to the expected matrices, number of samples, andfrequency of field QC samples (such as field blanks and field duplicates).

A field blank consists of sampling media that are shipped to the field and placedin a sampling train, but with no stack emissions pulled through the train. The fieldblank components are then recovered with the sampling train and returned to thelaboratory for analysis. Field duplicates are duplicate samples taken at the fieldsite: that is, duplicate stack samples taken with a dual probe and dual samplingtrains, for example, or duplicate aliquots of the same waste feed sample.

It is important to determine whether the proposed laboratory is capable ofanalyzing all sample matrices. Some laboratories do not analyze waste samples,and others do not analyze stack gas samples.

It is important to know the number of samples per matrix that the laboratory willanalyze so that the auditor can determine whether the laboratory has adequatecapacity to manage sample preparation, analysis, and reporting.

Check For: “ Whether the matrix is recorded on the laboratory audit checklist so thatthe auditor can determine whether the laboratory can analyze the matrix

“ Whether the approximate number of samples and field duplicates isrecorded on the laboratory audit checklist so that the auditor candetermine whether the laboratory has the capacity to analyze the numberof samples expected within the holding time period

Example Situation: Two laboratories are under contract for analysis: Laboratory A is to analyzestack gas samples, and Laboratory B is to analyze waste feed samples. Duringthe laboratory audit, Laboratory A receives a shipment of samples that containsgallon jars of a dark-colored, viscous material. The QA/QC manager realizesthat Laboratory A has received the wrong samples for analysis. The gallon jarsof dark-colored, viscous material are waste samples that should be analyzed byLaboratory B. He brings this error to Lois’ attention.



Example Action: Lois advises the QA/QC manager that the samples should be exchangedbetween the two laboratories so that the analysis can be correct. If holding timeshave expired before the correct samples are obtained, it may be necessary torepeat testing and sampling. Lois documents the situation that has occurred.

Notes:



2.2.4 Sample Handling, Traceability, and Holding Times



Explanation: Section 7.0 of the U.S. EPA Region 6 generic trial burn QAPP should identifyeach sample in addition to appropriate holding times for each analysis and anyrequired preservation techniques. All sample handling procedures for the trialburn must be described, including sample labeling, preservation, packing, shipping,laboratory, and field storage procedures. All documentation practices should bedescribed, including field logbooks, sample analysis request forms, laboratorycustody logbooks, and field chain-of-custody forms. Sample storage for archivepurposes must also be presented.

Check For: “ Whether the laboratory sample storage requirements and archivalrequirements in the trial burn QAPP are noted in the laboratory auditchecklist

“ Whether a place on the audit checklist is provided to record whetheractual laboratory performance on holding times and preservatives isconsistent with the approved trial burn QAPP

Example Situation: In reviewing information provided by the facility for the laboratory audit, Clarknotes that the trial burn QAPP states that the holding time for volatile organiccompounds (VOCs) is 28 days; however, Table 3-1 of the U.S. EPA 1990QA/QC Handbook states that the holding time is 14 days.

Example Action: During the audit, Clark brings the error to the attention of the laboratory projectmanager. The project manager agreed with Clark’s discovery. He told Clarkthat the laboratory followed the 14 day holding time. Clark noted the change andrequested the laboratory contact the facility before implementing any deviationsto the QAPP.

Notes:



2.2.5 Calibration Procedures and Frequency



Explanation: Section 8.0 of the U.S. EPA Region 6 generic trial burn QAPP presentscalibration procedures and frequencies for each analysis. Because this portion ofthe manual deals solely with laboratory audit concerns, the auditor should beconcerned about only portions of the trial burn QAPP dealing with calibration andfrequency for off-site analytical methods. Calibration requirements should bepresented in a concise, tabular format and should include (1) analytical method,(2) instrument, (3) frequency of initial and continuing calibrations, (4) acceptancecriteria, and (5) corrective action.

Calibration requirements are found in the analytical methods, such as SW-846. Trial burn QAPP calibration requirements should be consistent with, ormore stringent than, method requirements.

The laboratory audit checklist should contain calibration frequency, acceptancecriteria, and corrective action. The checklist should also include an itemregarding the traceability of standards to an U.S. EPA source or other certifiedstandard reference material.

Check For: “ Whether calibration requirements in the QAPP are consistent with, ormore stringent than, method requirements

“ Whether the calibration requirements are included in the laboratory auditchecklist

“ Whether the audit checklist includes a place for the QA/QC coordinatorto verify that calibration requirements have been met

“ Whether the traceability of standards is included in the laboratory auditchecklist

“ Whether the preparation and labeling of calibration standards areincluded in the laboratory audit checklist

“ Whether corrective actions are identified in the trial burn QAPP ifcalibrations fail criteria acceptance

Example Situation: In reviewing information provided by the facility for the laboratory audit, Loisnotes that the trial burn QAPP states that the calibration requirement of theinductively coupled plasma (ICP) instrument for metals analysis should include at



least four concentrations of standards for each analyte and a blank; however,U.S. EPA Method 6010A states that the calibration should include threestandards and a blank.

Example Action: Because trial burn QAPP requirements are more stringent than the methodrequirements, Lois finds the deviation to be acceptable.

Notes:



2.2.6 Analytical Procedures



Explanation: Section 9.0 of the U.S. EPA Region 6 generic trial burn QAPP should notinclude actual procedures for all analytical tests. Rather, it should summarizemethods, the quantitation limit for each analyte, and analytical method referencesfor all analytical tests. It should also detail any modifications to the methods, asreferenced. The auditor should have access to the methods to determine theapplicability of the method to the sample matrix and QA objectives. A detaileddescription of the selection of appropriate methods is provided in Section 3.4 of the U.S. EPA 1990 QA/QC Handbook.

Check For: “ Whether the methods summary includes sample preparation andanalytical methods and QC samples and criteria

“ Whether the methods listed in this section are appropriate for the samplematrix, as described in the approved QAPP and method summary in theanalytical reference

“ Whether the method chosen is capable of achieving the requiredquantitation limits for the project as specified in the approved QAPP

“ Whether the laboratory has demonstrated, for audit purposes, that anymodifications will enhance the analysis and will meet QC criteria. Theaudit team should have access to documents that demonstrate testmethod modification is acceptable (for example, replicate analyticalresults using the modification method). Section 2.1.9 of the U.S. EPA1990 QA/QC Handbook clearly indicates that an experienced chemistshould make these determinations.

Example Situation: In reviewing information provided by the facility for the laboratory audit, Clarknotes that the TBP states that the required reporting limit for lead in the wastefeed is 5.0 micrograms per liter, and the analytical method cited in the TBP isU.S. EPA Method 6010A. Although a reporting limit of 5.0 milligrams per liter isachievable for some ICP instruments, Clark determined that the instrumentpresently used by the laboratory is not capable of quantifying lead at thatconcentration.

Example Action: Clark asked that the facility either change the cited method to one more suitableto achieving the lower reporting limit (for example, U.S. EPA Method 7421 bygraphite furnace atomic absorption technique) or select another laboratory thathas the required capability.





Notes:



2.2.7 Internal Quality Control Checks



Explanation: Section 10.0 of the U.S. EPA Region 6 generic trial burn QAPP summarizesspecific internal QC checks required for each analytical method. A QC objectiveshould be associated with each QC check, as outlined in Section 5.0 of the U.S.EPA Region 6 generic trial burn QAPP, Section 2.2.5 of the U.S. EPA 1990QA/QC Handbook, and the approved QAPP..

Check For: “ Whether internal QC checks are listed for each method with theacceptance criteria in the trial burn.

“ Whether internal QC checks and the acceptance criteria for eachanalytical method are included in the laboratory audit checklist

Example Situation: In reviewing information provided by the facility for the laboratory audit, Loisnotes that the matrix spike recovery for chromium by U.S. EPA Method 6010 inthe trial burn QAPP is 75 to 125 percent, and the overall accuracy objective asexpressed by matrix spike recovery for the project is 50 to 150 percent.

Example Action: Because the method criteria are more stringent than the overall project objective,Lois finds the method criteria to be acceptable.

Notes:



2.2.8 Data Reduction, Data Validation, and Data Reporting



Explanation: For each analytical method, a brief description of the following items are includedin Section 11.0 of the U.S. EPA Region 6 generic trial burn QAPP:

• Data reduction scheme for nonroutine methods

• Listing of all final experimental data to be reported in the trial burn report

• Listing of all QC data to be reported in the trial burn report

This information is important to the laboratory auditor, because it will determinethe level of reporting that is required of the laboratory. Internal QC results mustbe evaluated with regard to overall QC objectives for the project (usuallyreferred to as validation). The data should be validated by a qualifiedenvironmental chemist.

Check For: “ Whether the laboratory employs the data reduction scheme fornonroutine methods discussed in the approved QAPP

“ Whether the laboratory lists experimental data in the trial burn reportaccording to the approved QAPP

“ Whether the laboratory plans to list all QC data in the trial burn reportaccording to the approved QAPP

“ Whether the laboratory lists target analytes with reporting limits andcorrect units for reporting in the trial burn report

“ Whether the laboratory indicates the specific use of blank data

Example Situation: In reviewing information provided by the facility for the laboratory audit, Clarknotes that the trial burn QAPP states that blank sample results will be used tocorrect concentration values for associated sample results. Section 2.1.11 of theU.S. EPA 1990 QA/QC Handbook states that correction of stack gas sampleresults for blank analysis is not recommended.

Example Action: Clark asks that the facility clarify this issue before samples are collected andanalyzed and that the facility notify the laboratory reporting staff of the change.

Notes:



2.2.9 Assessment Procedures for Accuracy and Precision



Explanation: Accuracy and precision are the assessment criteria used in determining whether data quality meets project objectives (see Section 13 of the U.S. EPA Region 6generic trial burn QAPP). Accuracy and precision are derived from equationslisted in Section 2.1.13 of the U.S. EPA 1990 QA/QC Handbook.

Check For: “ Whether the laboratory is using the correct equations for accuracy andprecision, as listed in the approved QAPP

“ Whether the laboratory correctly identifies each variable in the equations,as listed in the approved QAPP

“ Whether the laboratory is using acceptance criteria as identified in theapproved QAPP

Example Section: In reviewing information provided by the facility for the laboratory audit, Loisnotes that the laboratory states that the equation for accuracy is as follows:

Percent Recovery = 100 (found)/(amount found + amount spiked)

Example Action: The correct definition of percent recovery, as defined by Section 2.1.13 of theU.S. EPA 1990 QA/QC Handbook, is as follows:

Percent Recovery = 100 (found - native amount)/(amount spiked)

Lois asks that the laboratory correct the equation before samples are collectedand analyzed, and that the facility notify the laboratory staff of the change.

Notes:



2.2.10 Audit Procedures, Corrective Action, and QA Reporting


Guidance: U.S. EPA. 1990. “Handbook: QA/QC Procedures for Hazardous WasteIncineration.” CERI. Cincinnati, Ohio. U.S. EPA/625/6-89/023. January. Sections 2.1.14, 3.4, and 3.5.

Explanation: Section 14 of the U.S. EPA Region 6 generic trial burn QAPP should specify therequirements of internal audits (performed by the facility or contractors) andexternal audits (conducted by federal or state environmental agencies or agencycontractors). Audits may include the following:

• Systems audit of field and laboratory operations

• Instrument calibration check samples

• Blind spikes (amount known only to auditing agency) of blanksemivolatile organic sampling trains with POHC and surrogatePOHC

• Submittal of blind calibration check standards for each instrument

• Submittal of blind spikes of the POHC waste feed

• Submittal of U.S. EPA or National Institute for Standards andTesting reference samples for target analytes

• Audits of field records, analytical data, and other project records

• Overall data quality assessment, based on reported QC data

Check For: “ Whether the laboratory’s records indicate that laboratory systems auditshave been performed

“ Whether the laboratory audit was conducted by personnel independentfrom the trial burn team (see Section 2.1.4 of this component for moreinformation regarding selection of the laboratory audit team).

“ Whether the laboratory audit will be conducted while samples from thetrial burn are being prepared and analyzed



Example Situation: In reviewing correspondence provided by the facility for the laboratory audit,Clark notes that the trial burn field task leader will conduct the laboratory audit. Section 3.4 of the approved trial burn QAPP states that the laboratory audit willbe performed by personnel who are independent from the trial burn team.

Example Action: Clark asks that the facility revise their correspondence to require a person,independent of the project, conduct the audit before samples are analyzed.

Notes:



2.3 SCHEDULING THE AUDIT


Guidance: U.S. EPA. 1990. “Handbook: QA/QC Procedures for Hazardous WasteIncineration.” CERI. Cincinnati, Ohio. U.S. EPA/625/6-89/023. January. Section 3.4.

Explanation: The trial burn audit should be scheduled with each laboratory as soon as the fieldteam has determined the expected sample arrival date at the laboratory. Theaudit should be performed after the laboratory has received the first samples andbegun preparation and analysis. The best time for the audit is when a fewsamples have been prepared and are being analyzed. This approach allows theauditor to (1) verify the accuracy of tracking documentation, and (2) reviewcurrent procedures for preparation and analysis before it is too late to correctproblems without compromising the project.

Check For: “ Check frequently with the trial burn project manager regarding the fieldsampling events

“ Allow at least 2 to 10 days between sampling commencement and thelaboratory audit so that samples will be in the laboratory system. If morethan 10 days have lapsed from the last sampling date and the laboratoryaudit, samples will probably have been prepared and in the analytical orreporting stage.

“ Plan to be at the laboratory for 1 full working day, if more than one testmethod is being used. If the laboratory is analyzing stack gases, wastefeed, and ash for both organic and inorganic analyses, increase the planto 1½ working days. Remember that the complexity and initial findingsof the audit may cause the audit to extend for more than 1½ days.

“ Whether all key personnel identified in Section 2.1 of the U.S. EPA 1990QA/QC Handbook will be available during the tentative audit schedule

Example Situation: When scheduling the laboratory audit, Clark discovers that on the day chosen forthe laboratory audit, the laboratory’s designated project manager for the trial burnis away for meetings. The tentative scheduled day is only the fourth day afterthe beginning of sampling.

Example Action: Because it is early in the laboratory process, Clark chooses another day whenkey personnel are available.



Notes:



2.4 ASSEMBLING THE AUDIT TEAM


Guidance: U.S. EPA. 1990. “Handbook: QA/QC Procedures for Hazardous WasteIncineration.” CERI. Cincinnati, Ohio. U.S. EPA/625/6-89/023. January. Section 3.5.2.

Explanation: The composition of the audit team is very important to the success of the auditeffort. A complete team should consist of at least two individuals who areindependent of the trial burn team. The audit can be conducted with only oneauditor; however, two auditors reduces the possibility of errors ormisunderstandings.

At least one of the team members should be an analytical chemist (preferablywith direct experience in an environmental laboratory). A nonchemist may becapable of conducting a laboratory systems audit, but the chances of missingsubtle, important issues is greater. The team may consist of two chemists withdifferent backgrounds (for example, one organic and one inorganic). Bothmembers should be thoroughly familiar with the project-specific approved QAPP.

Check For: “ Whether the auditors are independent of the trial burn team

“ Whether at least one of the auditors is an analytical chemist (preferablywith direct experience in an environmental laboratory)

“ Whether both auditors have a thorough understanding of the trial burnQAPP

Example Situation: Lois, one of the auditors on the team, is an analytical chemist specializing ininstrumental techniques; Clark, the other auditor, specializes in samplingtechniques and field sample recovery. Lois finds a problem with the matrix spikebeing added to a metals analysis scheme after the sample is digested. Clarkdiscovers that volatile organic compounds (VOC) are being scheduled for thesame sample as semivolatile organic compounds (SVOC) and the volatiles aliquotis being taken after the semivolatiles aliquot.

Example Action: The expertise of both auditors was needed in this case. Lois recommends thatthe laboratory conform to the specified metals preparation procedures in themethod. Clark recommends that volatile samples be taken first, before theheadspace of the waste feed sample has been violated.



Notes:



2.5 PREPARING A LABORATORY-SPECIFIC CHECKLIST



Explanation: Printed checklists can be used to ensure that all systems have been fullyinspected and that all issues have been adequately addressed. Checklists can betailored to individual trial burn analytical methods and should include sections foreach of the items in the “Check For” list that follows. Appendix A, Part Two ofthe U.S. EPA 1988 RCRA Laboratory Audit Procedures provides an example ofa typical laboratory audit checklist. The guidance was designed for the auditingof groundwater monitoring programs; however, the same information isapplicable to the trial burn laboratory audit. The example was used to preparethe checklist used by U.S. EPA contractors and is included as Attachment A.The general checklist described here is adequate for use in performing alaboratory audit.

If more detail is required in the general checklist (for example, the auditors arenot chemists), additional checklists may be produced for each individualpreparation and analysis method that the laboratory uses during the trial burn. Information that must be included in individual method checklists is listed in Item2 of the “Check For” list that follows, and is also included in each method of theanalytical reference (such as U.S. EPA 1996 SW-846).

Check For: “ Whether the checklist contains a general laboratory practices section,including the following items:

“ Laboratory address and contacts“ QA manual review“ Personnel“ Laboratory equipment and supplies“ Receipt and storage samples“ Data handling and reporting

“ Whether each individual analytical method section includes the followingtopics and whether modifications to methods are being used:

“ Method number and reference“ Sample tracking documentation“ Apparatus and materials“ Reagents and standards“ Procedures (for preparation and cleanup methods, list the steps

for performing the procedure; for analysis, include instrument setup and calibration and procedures for analyzing samples)



“ QC requirements (list required QC with acceptance criteria andcorrective action requirements)

“ Whether the person is preparing individual method checklists is a chemistwith experience in an environmental laboratory

“ If the requirements of the trial burn QAPP and the referenced analyticalmethod differ, whether the approved trial burn QAPP requirements areused

Example Situation: Attachment A includes examples of general and individual method checklists. Increating the laboratory audit checklists, Lois plans to include specific informationregarding chromium analysis in waste feed, conducted by Method 6010 andrefers to U.S. EPA 1996 Test Methods for Evaluating Solid Wastes: LaboratoryManual, Physical/Chemical Methods (SW-846) Method 6010. Each section ofMethod 6010 describes the requirements and will contain the information listed inItem 2 of the “Check For” list.

Example Comments: Lois and Clark must decide whether the laboratory checklist should containdetailed method-specific sections based on past experience with the laboratory,past audit records of the laboratory, and their familiarity with the methods beingreviewed.

Notes:



3.0 CONDUCTING THE AUDIT



Explanation: The following sections describe each of the on-site audit activities on the basis ofinformation in guidance documents and actual experience of environmental QAchemists.

Check For: While conducting laboratory audits, auditors should conduct the following tasks:

“ Pre-audit briefing (Section 3.1)

“ Laboratory facility walkthrough (Section 3.2)

“ Checklist completion (Section 3.3)

“ Post-audit debriefing (Section 3.4)

The auditors should also conduct the following activities:

“ Whether the laboratory audit date has been confirmed with thelaboratory

“ Whether applicable laboratory checklists are available for the auditors

“ Whether key laboratory personnel will be available on the day of theaudit

“ Whether the auditors have verified that samples from the trial burn havebeen received by the laboratory and are being prepared and analyzed

Example Situation: In preparing for the laboratory audit, Clark—a nonchemist—completes thereview checklist to ensure that he is ready to begin the on-site audit.

Example Action: Clark notes that he has collected information regarding each of the precedingtopics. With his partner Lois—an experienced environmental QA chemist withfirst-hand laboratory audit experience—and this manual for information, Clarkmakes final preparations to travel to the first laboratory.

Notes:



3.1 CONDUCTING THE PRE-AUDIT BRIEFING



Explanation: Upon arrival at the laboratory, the audit team should conduct the pre-auditlaboratory briefing to:

• Introduce key laboratory personnel to the audit team• State the purpose of the audit• Describe the scope of the audit• Answer questions or address issues that laboratory personnel

have already encountered or expect to encounter during sampleanalysis

The following subsections describe each of the pre-audit laboratory briefingactivities.

Check For: “ Whether key laboratory personnel are present for the briefing (Section3.1.1)

“ Whether the auditors know the purpose and scope of the audit (Sections3.1.2 and 3.1.3)

“ Whether the auditors are ready to present trial burn QAPP changes, ifany, to the laboratory (Section 3.1.4)

“ Whether any unusual circumstances are expected surrounding thesample analysis (Section 3.1.4)

Example Situation: Upon arrival at the laboratory, the manager immediately escorts Lois and Clarkto the sample receiving area for the laboratory walkthrough.

Example Action: Lois and Clark should provide the laboratory key person with an audit agenda assoon as they arrive; that way, the key person will know that the pre-audit briefingis conducted prior to the laboratory walkthrough. Because the pre-auditlaboratory briefing is very important, Lois and Clark should insist that aconference room be secured for the briefing.

Notes:



3.1.1 Introducing Key Personnel



Explanation: The first purpose of the briefing is to introduce the audit team to all keylaboratory personnel. If possible, all key laboratory personnel, identified in thegeneral laboratory information (see Section 2.2.1 of this Component), shouldattend the briefing. Each person should indicate name, title, and overallresponsibilities with regard to trial burn samples.

Laboratory division managers (inorganic and organic) are often unavailableduring the briefing because of their operational duties. In such cases, anotherlaboratory manager present at the briefing should be delegated the responsibilityfor disseminating information to other laboratory managers. Auditors do notintend to inhibit the normal working activity of the laboratory, and they should tryto accommodate, within reason, the busy schedules of laboratory management.

Check For: “ Whether all key laboratory personnel are available

“ Whether all key laboratory personnel clearly understand the nature oftrial burn samples and their analysis

“ Whether all key laboratory personnel clearly understand their individualresponsibilities with regard to these trial burn analyses

Example Situation: During the introduction of personnel and responsibilities, Lois notes that theperson primarily responsible for implementing QC efforts is not present at thebriefing.

Example Action: Identify the personnel responsible for implementing the QC program and requesttheir presence at the briefing. If the person is not immediately available, schedulea time during the audit to meet with the person (as Lois does in this case).

Notes:



3.1.2 Stating the Purpose of the Audit



Explanation: Section 3.1 of this manual lists audit purposes, which should be stated in the pre-audit briefing.

Check For: “ Whether key laboratory personnel clearly understand the purpose of theaudit after the auditors have explained it to them

Example Situation: Laboratories are constantly audited by personnel from regulatory agencies andlocal clients and each audit has a different purpose. Regulatory agencies oftenaudit for compliance with regulations and require a stringent review of systemsand documentation. Client audits are often less rigorous and may require only alaboratory tour. Lois and Clark arrive at the laboratory and conduct a pre-auditbriefing. If the purpose is not stated, the laboratory does not know how torespond to questions or how much documentation to have available for review.

Example Action: In the pre-audit briefing, Lois and Clark state that the audit is in support of U.S.EPA’s trial burn oversight. To demonstrate compliance with applicableregulations and method procedures, the laboratory should be prepared to providethe full extent of documentation of sample receipt, preparation, analysis, andreporting.

Notes:



3.1.3 Describing the Scope of the Audit



Explanation: It is important to describe the scope of the audits by specifying the areas of thelaboratory facility that will be audited. The audit should be tailored to review onlyareas that will directly participate in the receipt, storage, preparation, and analysisof trial burn samples. In addition, areas of data reporting and sample disposalshould be reviewed. The relationship of the laboratory to the trial burn facilityshould be discussed. The order in which areas of the laboratory will be reviewedshould be discussed. If the laboratory is small (less than 20 personnel), the areaslisted in Section 3.2 of this component, rather than being separate locations in thelaboratory, may overlap. Typically, the audit starts at the point at which samplesare received by the laboratory and follows through each area of processing,ending with the data reporting section.

Check For: “ Whether key laboratory personnel are aware of laboratory areas that willbe handling trial burn samples

“ Whether each area reviewed has an analyst or supervisor present todiscuss the particular area

“ Whether key laboratory personnel understand their relationship with thefacility with regard to information transfer

“ Whether auditors and laboratory personnel have selected a route tofollow to cover all required areas

Example Situation: During the laboratory walkthrough, Lois and Clark discover that the auditedlaboratory has two senior staff members (a general manager and an operationsmanager) and five analysts that are located in a small section (three large rooms,plus offices) of a larger facility building. Samples are received directly into thesample preparation area (which includes inorganic and organic preparations),because it is located at the back entrance. One of the laboratory analysts is theacting sample custodian. The facility clearly has neither (1) separate, partitionedrooms for the areas listed in Section 3.2 of this component, or (2) dedicated staffmembers for each of the job descriptions listed in Section 2.1.1.2. of thiscomponent. The laboratory arrangement is not critical unless the actual area inwhich samples are received contains (1) solvent fumes (detectable by smell), (2) opened containers of waste samples (samples that are potentiallycontaminated heavily with organics and metals), or (3) rusty hoods that maycontribute to metals contamination when new samples are opened; Lois andClark do not observe any of these items.



Example Action: A laboratory analyst may act as the sample custodian if the responsibilities ofeach role are fully understood. In a small laboratory (staff of 15 to 20), it is notat all unusual for personnel to serve multiple functions. If multiple functions areserved, it is essential that the audit team verify that:

• Laboratory staff have received adequate training for multiplefunctions

• Laboratory training records completely document staff trainingand are up-to-date and comprehensive

• The laboratory QA officer is, and remains, organizationallyindependent of analysis and data generation or (if the QA officerserves as a backup analyst in one or more areas) that analternative QA review is obtained by another senior stafforganizationally independent of the analysis area

Lois and Clark verify that the laboratory analyst has also received samplecustodian training.

Notes:



3.1.4 Answering Questions and Addressing Issues From Laboratory Personnel



Explanation: To ensure a complete understanding of the project scope, it is important to allowlaboratory personnel to ask questions about the trial burn. Questions mayconcern a variety of subjects including (1) field sampling schedules, (2) changesin the number of samples taken, (3) sample condition upon receipt, and(4) discrepancies in sample receipt documentation. During the briefing, actionsitems—and the responsible personnel—should be identified.

Check For: “ Whether key laboratory personnel understand their roles in the trial burn

“ Whether action items—and the responsible personnel—are identified

“ Whether any action items require immediate attention that maycompromise data

Example Situation: During a laboratory audit, Clark discovers that the number of samples receivedsignificantly exceeds the initial estimate in the trial burn QAPP. Clark isconcerned that the increased sample load may overload the laboratory system,thereby causing the holding time to be exceeded and ultimately compromisingdata quality.

Example Action: Such issues are major and should be addressed immediately. Clark arranges aconference call with the facility trial burn manager and the laboratory QAmanager to resolve the issue.

Notes:



3.2 CONDUCTING THE WALKTHROUGH



Explanation: As discussed in Section 3.1.3, of this component, a walkthrough route should beselected during the briefing.

Check For: “ Whether the walkthrough route was determined during the briefing

“ Whether the checklist covers all areas reviewed during the audit

“ Whether the laboratory offers safety protection for areas requiring eyeprotection

“ Whether safety concerns are addressed: (1) gas cylinders arerestrained, (2) adequate hoods are available and are being usedappropriately to transfer solvents, prepare aliquots of samples, or performsample digests, (3) analysts are using safety glasses or other eyeprotection, and (4) appropriately labeled containers for waste disposal are available inthe lab

“ Whether laboratory housekeeping issues are addressed: (1) work areasare neat and uncluttered, (2) instruments are being operated underappropriate temperature control conditions, (3) laboratory functions areappropriately isolated, and (4) walkways are free of obstructions andclutter

The most logical route through the laboratory is as follows:

“ Sample receiving, storage, and custody area (Section 3.2.1)

“ Organic sample preparation laboratory (Section 3.2.2)

“ Organic analytical laboratory (Section 3.2.3)

“ Inorganic sample preparation laboratory (Section 3.2.4)

“ Inorganic analytical laboratory (Section 3.2.5)

“ Physical chemistry laboratory (Section 3.2.6)

“ Data reduction and reporting area (Section 3.2.7)



“ Sample archival and disposal point (Section 3.2.8)

Example Situation: From past audit experience, Lois has learned that unless the facility is containedin multiple buildings, the laboratory should accommodate the route described in“Explanation.” Laboratories sometimes are scattered in different buildings, andthe logistics of moving from one area to another in the prescribed order isdifficult.

Example Comments: Lois has also learned that the order of the laboratory walkthrough may beinfluenced by the times at which key personnel can be available to discusslaboratory operations and work flow. The order may be changed, provided thatall pertinent areas are covered.

Notes:



3.2.1 Sample Receiving, Storage, and Custody Area



Explanation: Section V of the example checklist provided in Attachment A of this componentcovers the requirements for trial burn sample receipt, storage, and custody. Thechecklist provides detailed questions that must be answered during the review ofthis area of the laboratory. The sample receiving area and refrigeration systemsshould be neat and orderly. There should be no broken or leaking samplecontainers exposed or solvent containers opened. The area should haveventilation hoods for opening sample shipping containers.

Check For: “ Whether the sample entry point of the laboratory is secure (for example,whether the exterior door has controlled access)

“ Whether the sample custodian is present and able to answer thequestions on the checklist

“ Whether samples are entered into the laboratory master log immediatelyupon receipt. If the laboratory master log is a manual system, goodpractices for laboratory notebooks are followed in making the sampleentries: (1) entries are made legibly, in black ink; (2) entries are signed orinitialed and dated; (3) entry errors are corrected properly -- single linestrike-through that does not obscure original data entry, with signature,date, and explanation for the correction

“ Whether trial burn samples have been entered into the laboratory systemand the documentation has been reviewed

“ How the laboratory work request is generated (for example, how doanalysts find out that samples have been received and that specificanalyses must be performed). If the sample custodian is responsible forgeneration of the work request documentation for each laboratory, thesample custodian knows which analyses are to be performed. Whenlaboratory work requests have been generated, they are reviewed toensure that correct analyses have been requested.

“ Whether the sample custodian can direct the auditor to the sample basedon the sample receipt and storage documentation generated by thelaboratory. The laboratory tracks the sample movement through thelaboratory (for example, when an analyst takes a sample out of storageto remove an aliquot, this information is recorded).



“ Whether the sample receiving area is neat and apparentlycontaminant-free

“ Whether samples are labeled adequately for identification: (1) labels areclear and unambiguous and (2) each sample is assigned a uniquelaboratory identifier that is associated with that sample throughout thelaboratory

“ Whether storage refrigerators are operating within required temperaturelimits and documented daily

“ Whether volatile organic sampling train samples are stored in a refrigerator separate from solvents, standards, or reagents

Sample storage refrigerators with identification numbers and temperaturerecords

Example Situation: Each laboratory has a unique tracking and documentation system. During anaudit, the sample custodian instructs Clark about internal laboratorydocumentation. One of Clark’s checklist items asks whether volatile samples arestored separately from nonvolatile or semivolatile samples. Using chain-of-custody records and documentation prepared by the laboratory, Clarklocates an individual sample container to determine whether it is a volatile sampleand whether it is stored in a refrigerated area with only volatile samples. Clarkdiscovers that volatile samples are stored in the same refrigerator as nonvolatilesamples.



Example Actions: Clark completes the checklist by placing an “X” in the “NO” column and entershis observation in the “Comment” column. Clark discusses the noncompliancewith the sample custodian and the QC manager.

Notes:



3.2.2 Organic Sample Preparation Laboratory

Regulations: No regulations are applicable to this section of the Manual.


Explanation: Organic sample preparation methods are found in SW-846 Volume 1B (3000series methods for organic analytes), Section 4.2 (Sample Preparation Methods). Sample preparation and sample cleanup methods are separate (in most cases)from the analytical methods. However, sample preparation methods (andcleanup methods, if applicable) are a part of the complete analytical method for aparticular analyte. Individual checklists prepared for each preparation methodwill describe the requirements to be reviewed.

The following activities are performed by the organic sample preparationlaboratory, and each should be accompanied by completed documentation (see“Check For” section).

• Receiving the sample from the laboratory sample custodian orfrom sample storage

• Weighing or measuring aliquots of the sample matrix forpreparation

• Preparing reagents, surrogate compounds, and standards

• Adding required spiking compounds or surrogate compounds asrequired by the method

• Performing required extractions/concentrations on samplematrices

• Placing the extract in the correct container with properidentification

• Secondary review of documentation by a supervisor or peer

Check For: “ Whether the laboratory documents sample transfer from storage to theappropriate person for preparation

“ Whether the laboratory has standard operating procedures (SOP) thatcorrespond to the analytical methods being audited. Whether the SOPsare available in the laboratory and are in use for trial burn samples



“ Whether the laboratory has logbooks or datasheets to document theweighing or measuring of the sample matrix

“ Whether the sample preparation logbook or data sheet indicates that thecorrect amount of sample was measured according to the preparationmethod

“ Whether the laboratory has a reagent or standard preparation logbookthat documents reagent and standard sources, solution preparation,preparation date, expiration date, and preparer’s initials

“ Whether the laboratory maintains maintenance and calibration logbooksfor instruments

“ Whether the laboratory logbook or datasheet indicates to which samplesspiking compounds or surrogate compounds have been added, theconcentration, and stock solution reference for traceability

“ Whether the laboratory logbook or datasheet indicates which and in whatquantity reagents are added to each sample

“ Whether the laboratory uses clearly labeled containers to hold theextracts and concentrates

“ Whether the laboratory logbook or datasheet indicates secondary reviewof the work

Example Situation: The trial burn QAPP requires that U.S. EPA Method 3542 be used forpreparation of samples generated by U.S. EPA Method 0010; this methodrequires separate extraction of each of the sampling train components andconcentration of each extract to a final volume of 5 milliliter (mL). The auditedlaboratory, however, usually combines all three of the fractions and concentratesthe extract to a final volume of 1 mL to enhance method detection limits. Loisdetermines that the combination of the extracts represents a deviation from theaccepted method.

Example Action: Because this method deviates from the one specified in the trial burn QAPP, Loisdiscusses the potential impact of the modification with laboratory personnel. Thisprocedure should be thoroughly described in the approved trial burn QAPP if thelaboratory is expected to follow the modified method. If the modification resultsin a negative effect (for example, the detection limits become higher than therequired limits), then the modification should be immediately stopped. If themodification results in a positive effect (for example, the detection limits becomelower than the required limits), then the effect should be noted in the commentsection of the checklist and audit report.



Notes:



3.2.3 Organic Analytical Laboratory



Explanation: Organic analytical methods are found in U. S. EPA 1996 SW-846 Volume 1B(8000 series methods for organic analytes). Organic analytical methods areseparate (in most cases) from preparation methods. However, the organicanalytical methods are a part of the whole method for the particular analyte orset of analytes. Individual checklists are available for each analytical method thatdescribe the requirements to be reviewed.

Organic analytes may be volatile (boiling point # 100EC), and the analyticalmethodology for the two classes of organic analytes is different. For volatileorganic analytes, the analytical methodology applied will be either purge and trap(for example, U.S. EPA Method 8260) or thermal desorption from a sorbent (forexample, the VOST coupled with either gas chromatography or gaschromatography/mass spectrometry (GC/MS). Analytical instrumentation forperforming VOC analysis is usually isolated from the organic preparationlaboratory and other instrumentation for performing SVOC analysis to avoidcontamination by organic solvents that are in common use in these areas. ForSVOC analytes, the analytical methodology applied will involve injection of aliquid solution (typically an extract of water, wastewater, sludge, or sorbent or adilution of a waste feed sample) into a gas chromatograph or a GC/MS.

Although each of the individual organic analytical methods has separaterequirements, the following routine activities are performed by the organicanalytical laboratory for most methods, and each should be accompanied bycompleted documentation (see “Check For” section).

• Receiving the sample, extract, or concentrate from the organicpreparation laboratory, the sample custodian, or sample storage,as appropriate for the individual sample

• Preparing reagents and standards

• Setting up and calibrating instrumentation

• Determining method detection limits for each analyte

• Analyzing multipoint calibration samples, calibration checksamples, and blanks



• Analyzing other QC check samples required by the analyticalmethod

• Reducing bench-level data

• Evaluating bench-level data

• Performing a secondary review of documentation by asupervisor or peer

Check For: “ Whether the laboratory documents sample transfer from the preparationlaboratory or from sample custody to the appropriate analyst

“ Whether the laboratory has appropriate storage for standards (forexample, standards are stored separately from samples and volatilestandards are stored separately from samples and from semivolatilestandards or samples)

“ Whether the laboratory has a reagent or standard preparation logbook ordatasheet that documents the preparation methodology for reagents andstandards, the preparation date, the expiration date, preparer’s signatureor initials, and the source of the material for traceability. The preparationof reagents and standards may be included in the preparation laboratorylogbooks or datasheets.

“ Whether (1) the laboratory has SOPs for the methods being audited,(2) the SOPs are available in the laboratory, and (3) the SOPs are in usefor the methods being audited

“ Whether instruments are set up and calibrated correctly for the methods

being audited. Calibration data receive both primary and secondaryreview before a calibration curve is used.

“ Whether the laboratory has instrument maintenance logs to documentany maintenance activities for analytical instrumentation and whetherthese logs are accurate, up-to-date, and signed

“ Whether the laboratory has method detection limits for each analyte thatis less than or equal to reporting requirements in the trial burn QAPP foreach matrix analyzed

“ Whether the laboratory analyzes QC samples required by the method atthe proper frequency, and whether analytical results meet methodacceptance criteria



“ Whether the laboratory has internal QC acceptance criteria by which toevaluate QC sample results (for example, control charts are accurateand current)

“ Whether the laboratory QC acceptance criteria for each QC sample typeis consistent with, or more stringent than, project trial burn QAPPrequirements

“ Whether the laboratory analyst reduces the data at the bench to the finalreporting units. If not, who is responsible for generating the finalreporting units for each measurement?

“ Whether the laboratory analyst, QA officer, or supervisor reviews all QCdata and determines data acceptability relative to the method and/or trialburn QAPP acceptance criteria. Which procedure does the laboratoryfollow for QC data that fails to meet acceptance criteria?

“ Whether data are reviewed by a peer or supervisor or QA officer beforesubmission to the data reporting section of the laboratory

“ At what stage of the analysis/reporting process is the data set reviewedfor completeness?

“ Whether sample holding times are tracked in the laboratory to ensure thatall samples are prepared/analyzed within holding times

“ Whether a logbook for sample analysis is maintained daily and signed bythe analyst



GC/MS for Volatile Organic Analysis with Purge and Trap Apparatus

Example Situation: One requirement for VOC analysis by GC/MS is the daily analysis of acalibration check sample that must meet method acceptance criteria beforesample analysis is performed. Acceptance criteria for calibration check samplesare available in the U.S. EPA 1996 SW-846 method, the laboratory SOP, the trialburn QAPP, and the method-specific laboratory checklist. The correctcalibration procedure must be immediately implemented. During the audit, Clarkverifies that calibration check samples are taken and analyzed daily in methodaccordance criteria.

GC/MS for Semivolatile Organic Analysis with Autosampler



Example Action: If the laboratory fails to perform the required calibration check or if thecalibration check fails to meet acceptance criteria but samples are analyzed,these items should be noted in the laboratory checklist.

Notes:



3.2.4 Inorganic Sample Preparation Laboratory



Explanation: Inorganic sample preparation methods are in U.S. EPA 1996 SW-846 Volumes1A (3000 series methods for metals) and 1C (9000 series methods for nonmetals)(U.S. EPA 1994). Most of the metals preparation methods are separate fromanalytical methods; however, nonmetals preparation methods are included in theoverall analytical method for the particular analyte. Individual checklistsprepared for each preparation method will describe the requirements to bereviewed.

The inorganic preparation laboratory performs the following activities, each ofwhich should be completely documented (see “Check For” section).

• Receiving the sample from the laboratory sample custodian

• Receiving the laboratory work request

• Weighing aliquots of the sample matrix for preparation


• Adding required spiking compounds, when required by themethod

• Performing acid digestions or distillations on sample matrices

• Containerizing the digest or distillate with proper identification

• Performing a secondary review of documentation by supervisoror peer

Check For: “ Whether the laboratory documents sample transfer from storage to theappropriate person for preparation

“ Whether the laboratory has SOPs that correspond to the analyticalmethods being audited

“ Whether the laboratory has logbooks to document the weighing of thesample matrix



“ Whether the preparation logbook indicates that the correct amount ofsample was measured, in accordance with the preparation method

“ Whether the laboratory has a reagent or standard preparation logbookthat documents reagents and standards recipes, last preparation date, andpreparer’s initials

“ Whether the laboratory logbook indicates the samples to which spikingcompounds have been added and the concentration

“ Whether the laboratory logbook indicates the reagents that are added toeach sample and the amount

“ Whether the laboratory uses clearly labeled containers to hold digestsand distillates

“ Whether the laboratory logbook reflects a secondary review of the work

“ Whether instrument calibration logbooks are maintained

Example Situation: One requirement for the digestion of samples for metals analysis is the addition ofnitric acid to the sample. This information is available in both U.S. EPA 1996SW-846 and the laboratory checklist. During an audit, Lois discovers that thelaboratory uses sulfuric acid instead of nitric acid for this procedure, which is adeviation from the method.

Example Action: If the auditor is not experienced enough to determine the acceptability of thismodification, an experienced inorganic chemist should be consulted immediately. The chemist should determine that the use of sulfuric acid may produce anunacceptable result, because sulfate compounds of many metals are less solublethan their nitrate form. Lois advises the laboratory QC manager that theprocedure should be immediately corrected; she also notes the problem on thechecklist and in the audit report.

Notes:



Acid digestion hood associated with inorganic sample preparation



3.2.5 Inorganic Analytical Laboratory



Explanation: Inorganic analytical methods are in U.S. EPA 1996 SW-846, Volumes 1A(Method 6010A and 7000 series methods for metals) and 1C (9000 seriesmethods for nonmetals). Most of the metals analytical methods are separatefrom preparation methods; however, nonmetals analytical methods are included inthe overall method for the particular analyte. Individual checklists are availablefor each analytical method that will describe the requirements to be reviewed.

Although each of the individual analytical methods has separate requirements, theinorganic analytical laboratory performs the following routine activities for mostmethods. Each activity should be completely documented (see “Check For”section).

• Receiving the sample digest or distillate from the inorganic

preparation laboratory

• Receiving a laboratory work request from the sample custodianor other source


• Setting up and calibrating instrumentation

• Obtaining method detection limits for each analyte

• Analyzing calibration checks and blanks

• Analyzing other method-required QC samples

• Reducing bench-level data

• Evaluating bench-level data




Check For: “ Whether the laboratory documents the sample digest or distillate transferfrom the preparation laboratory to the appropriate person for analysis

“ Whether the laboratory receives a work request prior to sample receipt

“ Whether the laboratory has a reagent or standard preparation logbookthat documents reagents and standards recipes, last preparation date, andthe preparer’s initials (may be incorporated into preparation laboratorylogbooks)

“ Whether working standards can be traced to certified stock standards

“ Whether sample analysis logbooks are maintained and signed by analysts

“ Whether the laboratory has SOPs for the analytical methods beingaudited

“ Whether these SOPs are accessible and are being used in the laboratory

“ Whether the instrumentation is set up and calibrated in accordance withthe methods being audited

“ Whether the laboratory has method detection limits for each analyte thatare less than, or equal to, the reporting requirements established in thetrial burn QAPP for each matrix for which analysis is conducted

“ Whether the laboratory analyzes the method-required QC samples at theproper frequency

“ Whether the laboratory has QC acceptance criteria to use in evaluatingQC sample results

“ Whether laboratory QC acceptance criteria for each QC sample type areconsistent with, or more stringent than, trial burn QAPP requirements

“ Whether the laboratory analyst reduces data at the bench to the units andreporting limits described in Attachment A (if not, find out who isresponsible for this task)

“ Whether the laboratory analyst, QC officer, or supervisor reviews all QCdata and determines its acceptability on the basis of acceptance criteria

“ Whether data are reviewed by a peer or supervisor before submittal tothe data reporting section of the laboratory



Example Situation: One requirement for the analysis of metals by ICP in accordance with Method6010A is that an initial calibration verification sample be analyzed followingcalibration, and that a calibration verification sample be analyzed for 1 of every10 samples. This information is available in U.S. EPA 1996 SW-846 and thelaboratory checklist. During the audit, Clark discovers that the laboratoryanalyzes calibration verification samples for 1 of every 20 samples.

Example Action: Clark advises the laboratory QC manager that the procedure should beimmediately corrected; he also notes the deviation on the checklist and in theaudit report.

Notes:

Mercury analysis



Inductively coupled argon plasma emission spectrometer

Atomic absorption spectrometer



3.2.6 Physical Parameter Laboratory



Explanation: Methods for the determination of physical parameters (for example, Britishthermal unit [Btu], chloride content, oil and grease content, ignitability, sulfurcontent, density, ash, and moisture content) are found in SW-846 for some of theparameters and in the ASTM series of methods. The methods as writtenincorporate both sample handling and analysis. Individual checklists are availablefor each analytical method that describe the requirements to be reviewed.

Each of the individual analytical methods has separate requirements and, in thetypical laboratory that performs the determination of waste fuel physicalparameters, physical parameter determination is usually performed in a laboratoryarea removed from the location of inorganic and organic analyticalinstrumentation.

The following routine activities are conducted by the physical parameterdetermination laboratory for most of the methods used, and each should beaccompanied by completed documentation (see “Check For” section).

• Receiving the sample from the laboratory sample custodian orfrom sample storage

• Receiving a work request in the laboratory to ensure that thestaff understands which analysis should be performed

• Weighing and measuring aliquots of the sample matrix forpreparation; preparing composites of waste fuel matricessampled throughout the duration of a sampling run; homogenizingwaste fuel samples prior to removing an aliquot for analysis, anddiluting the waste fuel matrix for organic analysis

• Preparing the reagents, surrogate compounds, and standards

• Adding the required spiking compounds or surrogate compounds,as required by the method

• Performing required dilutions on homogenized waste fuel matrix

• Placing the sample in the correct container with properidentification




Check For: “ Whether the laboratory documents sample transfer from storage to theappropriate person for preparation and analysis and whether extremelyviscous waste fuels are stored appropriately under ambient conditionswith restricted access

“ Whether (1) the laboratory has SOPs that correspond to the analyticalmethods being audited; (2) the SOPs are available in the laboratory, and(3) the SOPs are in use for trial burn samples

“ Whether the laboratory has logbooks or datasheets to document thesample matrix compositing, aliquoting, weighing, or measuring

“ Whether the laboratory has appropriate facilities for safe handling oflarge quantities of waste fuel. If heating of extremely viscous waste fuelsamples is required before a composite can be prepared, the matrices areheated safely in a hood

“ Whether the sample preparation logbook or datasheet indicates that the

correct sample amount was measured according to the preparationmethod

“ Whether (1) the laboratory has instrument run logs and instrumentmaintenance and calibration logs for each of the analytical instruments inuse; (2) these logs are maintained according to good laboratory practicefor maintaining a notebook; and (3) the logs are current

“ Whether the laboratory has a reagent or standard preparation logbookthat documents reagents and standards sources, solution preparation,preparation date, expiration date, and the preparer’s initials

“ Whether the laboratory logbook or datasheet indicates to which samplesspiking compounds or surrogate compounds have been added and theconcentration

“ Whether the laboratory logbook or datasheet indicates which and in whatquantity reagents are added to each sample

“ Whether the laboratory uses clearly labeled containers to hold samples

“ Whether the laboratory logbook or datasheet indicates secondary reviewof the work



Example Situation: Waste fuel samples must be diluted, often by a factor of 1,000 or more, toperform a qualitative VOC analysis without saturating analytical instrumentationand to bring the analytes that are present into an appropriate range for thecalibration curve. While performing an audit, Lois notes that a 1,000-fold dilutionof a composited waste fuel yields a chromatographic peak for benzene that is stillsaturated.

Example Action: No meaningful analytical results can be reported on the basis of saturatedchromatographic peaks. To obtain meaningful analytical results for the wastefuel composite, solvent blanks must be analyzed on the analytical instrument untilthe absence of benzene carryover is demonstrated. Lois discusses this issue withthe laboratory QC manager and advises that the laboratory personnel dilute acomposited waste fuel sample to an appropriate level (for example, 10,000-fold) and analyze it to obtain quantitative values for benzene.

Notes:



BTU calorimeter

BTU Parr bombs



3.2.7 Data Reduction and Reporting Procedures



Explanation: Data reduction and reporting procedures are in U.S. EPA 1996 SW-846, ChapterOne, Section 4.4.6 (Data Handling). The section of the laboratory responsiblefor gathering all analytical, sampling, and QC data should report the limitsspecified in the trial burn QAPP; and assemble the data package deliverable.

Supporting documentation should include, at a minimum, the following items:

• Laboratory name and address

• Sample information (including unique sample identification,sample collection date and time, sample receipt date, and samplepreparation and analysis dates)

• Complete field and laboratory chain-of-custody records

• Analytical results reported with an appropriate number ofsignificant figures

• Detection limits that reflect dilutions, interferences, or correctionfor equivalent dry weight

• Method reference

• Appropriate QC results for each batch of samples included in thereport

• Data qualifiers with appropriate references

• Written narrative about the quality of the results

Check For: “ Whether the laboratory report contains the preceding information

“ Whether the laboratory uses computer-aided reporting

“ Whether computer software programs for data reduction are periodicallyverified with hand-calculated results

“ Whether a manager or other senior laboratory staff member writes thecase narrative



“ Whether the case narrative provides information regarding any QCcheck that does not meet acceptance criteria established in the trial burnQAPP

“ Whether the entire data package is reviewed by a manager or othersenior laboratory staff member before submittal to the client.

Example Situation: During an audit, Lois discovers that all chloride results are hand-entered into thelaboratory information management system by a nontechnical clerk and thatfollowing entry, the data are reported without a secondary review by a technicalstaff member.

Example Action: Lois notes in the checklist and the audit report that data are reported without asecondary technical review; she also advises the laboratory QC manager that thispractice should be immediately addressed.

Notes:



3.2.8 Archival and Disposal of Samples



Explanation: Sample archival is important in the event that the facility, based on initial reportedresults, needs follow-up or different analyses. Because every laboratory has itsown SOPs for archival and sample disposal, the requirements for each laboratorybeing audited should be noted. Some laboratories require that the unused samplebe shipped back to the sampling source.

Check For: “ Whether the laboratory has a standard procedure for archival anddisposal of samples (note the requirement for each laboratory.)

“ Whether the laboratory requires that the sample be sent back to thesource

“ Whether the laboratory has a contractor available to dispose of unusedsamples in accordance with applicable state and federal regulations

“ Whether the laboratory keeps records of sample disposal

“ Whether the laboratory retains samples for a specified period of timeunder appropriate storage conditions (for example, refrigerated orambient)

“ Whether the laboratory will make special provisions if the facility wantsthe samples archived (1) longer than the standard time, or (2) undernonstandard conditions

Example Situation: During an audit, Clark notes that the reported result for chlorine in the waste feedis 10 times greater than the results expected on the basis of prior analyses, andhe questions the current laboratory findings. Clark discusses the possibility ofreanalysis with the laboratory QC manager.

Example Action: If the sample matrix (waste feed) is still available for analysis in the laboratory,the facility may request a reanalysis. Most laboratories do not keep field samplesfor more than 30 days after the report is submitted, and the sample is not alwayskept in cold storage. Sample availability and condition, upon request forreanalysis, may determine whether reanalysis is feasible. Clark locates thesample in question in archival, reviews its storage condition, evaluates the holdingtime that has elapsed, and determines that reanalysis is feasible and will producevalid results. He indicates to both the facility trial burn manager and thelaboratory QC manager that sample reanalysis is advisable.



Notes:



3.3 COMPLETING THE AUDIT CHECKLIST

Regulations: No regulations are applicable to this section of the manual


Explanation: As stated in Section 2.5 of this component, the use of printed checklists ensuresthat all systems are fully inspected and that all issues have been adequatelyaddressed. It is important that the audit team complete the checklist by handbefore leaving the laboratory. This practice ensures that, if the auditors haveomitted any items, the laboratory can respond before the auditors leave. Completing the checklist also enables the auditors to discuss deficiencies ordiscrepancies noted before leaving the laboratory.

Check For: “ Whether the auditors have completed all checklist sections (Section3.3.1)

“ Whether the auditors failed to see any part of the laboratory system thataffects project sample analysis (Section 3.3.2)

“ Whether the auditors failed to obtain any information from the laboratoryconcerning any issue (Section 3.3.2)

“ Whether the auditors noted any deficiencies or discrepancies that requireresolution (Sections 3.3.3 and 3.3.4)

Example Situation: When the audit team begins to prepare the audit report, they discover that theydid not record on the checklist the name or telephone number of the laboratoryQC officer. Lois and Clark need clarification on a particular issue that requirescontact with the laboratory QC officer.

Example Action: Lois calls the laboratory to identify the QC officer and to obtain his/her telephonenumber before the report is complete. Because they failed to obtain thetelephone number earlier, an additional step to the auditing process must beadded.

Notes:



3.3.1 Answering the Checklist Questions



Explanation: The auditor may also include additional comments regarding positive aspect ofthe laboratory audit, describing procedures that the laboratory performsexceptionally well.

Upon return to the office, auditors should review all checklists that werecompleted during the course of the audit. If the audit was performed by a teamof two individuals, each auditor will have a completed checklist. Although apreliminary review of the checklists was performed before leaving the laboratory,it is still possible that some area was overlooked. A final review of thechecklists, together with the U.S. EPA Region 6 generic trial burn QAPP, shouldbe performed to ensure that all checklist questions are answered, all negativeresponses have explanatory comments, and all other questions have beenanswered, and any discrepancies between areas audited and the U.S. EPARegion 6 generic trial burn QAPP have been resolved.

Check For: “ Whether comments require clarification or amplification after some timehas elapsed after the audit

Example Situation: While completing an audit checklist, Clark indicates a negative response to thechecklist question (below) and cross-references the comment with a number. The numbering system he uses includes the section number followed by anumerical sequence beginning with one.

SECTION IV GENERAL LABORATORY SUPPLIES AND EQUIPMENT

Requirement Yes No NA Comments (Explain all negativeresponses)

Are all reagents and IV-1 IV-1 Reagents and solutions weresolutions labeled to clearly labeled; however, theindicate identity, expiration date was not included.concentration, storagerequirements,preparer’s name,preparation date, andexpiration date?

Example Action: Clark completes the checklist as the audit is conducted so that all findings arerecorded. The checklist should be completed as indicated above. For responsesthat do not require a comment, the auditor may use an “X” or a check mark.



Notes:



3.3.2 Noting Omissions



Explanation: Before the auditors conduct the debriefing (see Section 3.4 of this component),they should note and review any omissions. The appropriate laboratory sectionshould be re-reviewed to include the omission. The omission may be covered bya question to the laboratory QC officer or supervisor.

Check For: “ Whether the auditors noted any areas of the laboratory system that weremissed during the walkthrough

“ Whether the omission can be resolved by asking a question or whetherthe audit team must return to the laboratory area for the review

“ Whether the auditor completed the question on the checklist after the re-review

Example Situation: In preparation for the audit debriefing, Lois and Clark discover that they did notsee the calibration record for the mercury autoanalyzer.

Example Action: Lois and Clark request that the laboratory supervisor bring the record to them,and alternatively, auditors may ask to return to the inorganic analytical laboratoryto see the record. After reviewing the record, Lois completes the question on thechecklist.

Notes:



3.3.3 Noting Deficiencies



Explanation: Before the auditors conduct the debriefing (see Section 3.4 of this component),they should note and prepare to discuss any deficiencies. Deficiencies are areasthat do not meet either method-specific or trial burn QAPP requirements. Theseissues should be brought to the attention of the key personnel present for thedebriefing.

When audit checklists have been completed and reviewed, areas may exist inwhich checklist questions were answered in the negative and are accompaniedby comments on the checklist. There may be other observations of deficienciesfrom the laboratory walk-through that do not correspond directly with a specificarea of the checklist. Each auditor should compile a list of deficiencies, andassess whether they have or do not have an impact on the quality of the data. Evaluating whether a deficiency impacts the data quality may require reviewingthe observation against the approved QAPP, as well as the methods andprocedures being used.

Deficiencies that have an impact on the quality of the data encompass thefollowing concerns:

• Inconsistency with requirements of the U.S. EPA Region 6generic trial burn QAPP

• Insufficient QC, based on U.S. EPA 1990 QA/QC Handbook• Major unauthorized modifications of analytical methods cited in

the U.S. EPA Region 6 generic trial burn QAPP

Check For: “ Whether areas of deficiencies were noted and, if so, the impact on dataquality

“ Whether auditors have proof of deficiencies

“ Whether all negative responses on the checklist have a commentexplaining the response

“ Whether any other laboratory deficiencies noted in the laboratory walk-through are thoroughly documented

Example Situation: During the audit, Lois and Clark discover that the laboratory calibrates themercury analyzer with two calibration standards and a blank. U.S. EPA Method7471A, Section 7.3, states that four standards and a blank must be used for initial



calibration of the mercury analyzer. Section 8.0 of the U.S. EPA Region 6generic trial burn QAPP, states that instruments will be calibrated in accordancewith U.S. EPA 1996 SW-846 methods.

Example Action: Lois and Clark note this deficiency and are prepared to cite the references inSW-846 and the trial burn QAPP to key laboratory personnel in the debriefing. As documentation of the deficiency, Clark makes a copy of the instrument runlog signed by the analyst and showing the sequence of analyses.

Notes:



3.3.4 Noting Additional Questions



Explanation: During the audit, the audit team may remember other questions regarding sampleanalysis that do not directly affect this project. These questions may concernother services that the laboratory provides that may be of use on future projectsor on future work for this project. The questions may also concern the theory ofspecific techniques or new developments in techniques that add to the auditors’understanding.

Check For: “ Whether auditors noted any other areas requiring clarification that are

not critical to the project

Example Situation: During the audit, Lois and Clark discuss the relevance of using massspectrometry with ICP to enhance the analysis of trace metals. The technique isnot directly relevant to the project, because it is not referenced in the trial burnQAPP; however, it is important to continually investigate new techniques or ideasto further the personal education of the team.

The audit team may have read publications that deal with high pH digestion(alkaline digestion) used for hexavalent chromium analysis. The laboratory maybe able to provide first-hand information concerning practical uses of thistechnique for future work on this project.

Example Actions: No action is required; however, the information obtained can be used to enhancefuture projects.

Notes:



3.4 CONDUCTING THE AUDIT DEBRIEFING



Explanation: After checklist completion, the audit debriefing should be conducted and shouldinclude the following items:

• Key laboratory personnel meet with the audit team (samepersonnel as in the briefing, see Section 3.1)

• State whether the purpose of the audit was met (see Section

3.1.2)

• Describe positive and negative initial findings (see Section 3.3.2)

• Discuss the required follow-up by the laboratory (see Sections3.3.3 and 3.3.4)

Because all of these items, except the last one, are discussed in other sections, nofurther detailed discussion is necessary. It is important to discuss the requiredfollow-up by the laboratory. Deficiencies should be categorized by priority:(1) major concerns which compromise data quality, or (2) minor concerns whichdeviate from prescribed methods but do not compromise data quality. Thelaboratory should address concerns in writing, providing documented proof of thecorrective action taken. Auditors should explain to the laboratory what will beexpected regarding follow-up on all issues.

Check For: “ Whether key laboratory personnel are present for the debriefing

“ Whether the audit satisfied the purpose and scope

“ Whether the auditor presents deficiencies to laboratory personnel

“ Whether the auditor has references to support the deficiencies

“ Whether the audit team has a plan for laboratory follow-up

“ Whether auditors or laboratory personnel have other questions



Example Situation: During an audit, Lois and Clark realize that the laboratory failed to analyze amatrix spike with a batch of waste feed samples. Without matrix spike data, thedata reviewer cannot judge the potential effect of matrix interference. Especiallyin an organic matrix, the potential for matrix interference is high; without spikeevaluation, the interface effect cannot be determined.

During an audit, Lois and Clark note that laboratory results for impinger solutionsare in milligrams per liter (mg/L) instead of nanograms per liter, as required bythe trial burn QAPP. The results are correctly calculated to mg/L, so Lois andClark are not overly concerned. Laboratories are often able to program thelaboratory information system to report in different units, and the laboratoryshould verify that the change is implemented correctly.

Example Action: In the first example, Lois and Clark consider this deficiency to impact data qualityand require follow-up by the laboratory. The laboratory may offer data fromanother batch of samples from the same project or another project with a similarmatrix.

In the second example, Lois and Clark request that the laboratory follow up bycorrecting the error and documenting the corrective action taken.

The issues presented above should be thoroughly discussed with the keypersonnel present at the debriefing. If the issue is relevant to a particular area ofthe laboratory, the supervisor of that group may be asked to attend the debriefing. Most issues will already have been addressed at the point of discovery. Keyissues should be brought up again, along with the most efficient solution to theproblem.

Notes:



4.0 POST AUDIT ACTIVITIES



Explanation: The following sections describe each of the post audit activities based on(1) information in guidance documents listed above, and (2) actual experience ofenvironmental QA chemists.

Check for: “ After the audit debriefing with laboratory staff, is the audit team takingadequate notes and descriptive material from the laboratory to prepare adetailed audit report?

The following tasks should be completed away from the laboratory site byauditors:

“ Review checklists prepared after the laboratory walk-through andcompile a list of deficiencies (Section 4.1)

“ Define concerns that have been uncovered during the audit (Section 4.2)

“ Prepare the audit report (Section 4.3)

Example Situation: The auditors agree that the laboratory can carry out the minimum requirementsof the project, but were distracted by the untidiness and overall disorganization ofthe facility.

Example Action: Assimilating objective information is the key to a successful audit. The auditorsmust decide if the observations were merely housekeeping issues, health andsafety issues, or if the observations are indicative of underlying problems thatmay affect the overall validity of the analytical data.

Notes:



4.1 REVIEWING AUDIT INFORMATION



Explanation: The printed checklists in Attachment A are in a question format. Each auditorwill answer each question with one of three responses: Yes, No, or NotApplicable. In addition, in the checklist column for comments, each auditor willprovide a comment to identify or clarify the problem for each negative response. The auditor may also include additional comments regarding positive aspects ofthe laboratory audit, describing procedures that the laboratory performsexceptionally well.

On returning to the office, auditors should review all checklists that werecompleted during the course of the audit. If the audit was performed by a teamof two individuals, each auditor will have a completed checklist. Although apreliminary review of checklists was performed prior to leaving the laboratory, itis still possible that some area was overlooked. A final review of checklists,together with the trial burn QAPP, should be performed to ensure that allchecklist questions are answered, all negative responses have explanatorycomments, all other questions have been answered, and any discrepanciesbetween audited areas and the trial burn QAPP have been resolved.

When audit checklists have been completed and reviewed, areas may exist inwhich checklist questions were answered in the negative and are accompaniedby comments. Other observations of deficiencies from the laboratory walkthrough may not correspond directly with a specific area of the checklist. Eachauditor should compile a list of deficiencies, ranking the deficiencies either asmajor (having an impact on data quality) or minor (not having an impact on dataquality). Deciding whether a deficiency represents a major or a minor concernmay require reviewing the observation against the trial burn QAPP, as well asmethods and procedures being used.

The following deficiencies, if present as applied to the activity, procedure,method, or documentation being reviewed, would be considered major:

• Inconsistency with requirements of the risk burn plan for thefacility

• Inadequate QC, based the U.S. EPA 1990 QA/QC Handbook

• Major modifications of analytical methods cited in the trial burnplan



Check for: “ Do all checklist questions have a response?

“ Do all negative responses have a comment explaining the response?

“ Are the comments correctly cross-referenced to the response?

“ After some time has elapsed after the audit, do the comments requireclarification or amplification?

“ Do all negative responses on the checklist have a comment explainingthe response?

“ Are any other laboratory deficiencies noted in the laboratory walkthrough thoroughly documented?

“ Are all deficiencies compiled into a list?

“ Are deficiencies considered to be major or minor based on the trial burnQAPP and actual methods?

Example Situation: Upon review of the audit checklist on the day after returning to his office, Clarkauditor realizes that a cryptic comment, “Problems with calibration,” does notprovide sufficient detail to show exactly what the problem was and howlaboratory practices for calibration failed to satisfy trial burn QAPPrequirements.

Example Action: The auditor may recall sufficient information to provide an detailed explanation ofthe nature of the problem (as Clark does in this case), or a call to the laboratorycontact person or one of the key personnel may be required to provide sufficientclarification so that the auditor can clarify or amplify his comment.

Notes:



4.2 ANALYSIS OF DEFICIENCIES



Explanation: In the preparation of the final audit report, the audit team must summarizechecklist comments and categorize deficiencies as major or minor.


C Inconsistency with requirements of the risk burn plan for thefacility

C Inadequate quality control, based on the U.S. EPA 1990 QA/QCHandbook

C Major modifications of analytical methods cited in the trial burnplan

The laboratory must respond and address major concerns raised by the auditteam.

Minor concerns are laboratory deficiencies that do not have an impact on dataquality. The laboratory may respond but is not required to do so.

Check for: “ Are all laboratory deficiencies compiled into a list by each auditor?

“ Are the deficiencies considered to be major or minor based on the trialburn QAPP and actual methods?

The following subsections describe these subjects in more detail:

“ Comparing findings between audit team members (Section 4.2.1)

“ Identifying major concerns (Section 4.2.2)

“ Identifying minor concerns (Section 4.2.3)

“ Preparing preliminary comments (Section 4.2.4)

Example Situation: In reviewing the laboratory’s SOPs and in discussing with laboratory keypersonnel the laboratory’s practices and procedures for staff training, Lois andClark discover that the laboratory training practice is as follows: (1) an analyst is



taught a given procedure by an experienced senior analyst, (2) the analystperforms the procedure under the supervision of the senior analyst for a specifiedperiod of time, and (3) when the senior analyst is satisfied with his performance,the trainee may perform the procedure unsupervised. However, no central fileexists in the laboratory that contains written documentation that Analyst A hasreceived training in Procedure X and has completed this training satisfactorily.

Example Action: If Analyst A has completed this process to his trainer’s satisfaction, he isperforming the procedure correctly and consistently with the laboratory’s SOPs. The laboratory should have an up-to-date, central file that providesdocumentation to certify which analyst has been trained in which procedures, butLois and Clark conclude that the lack of a central file does not have an adverseeffect on analytical data. Lois and Clark advise the laboratory manager that itwould be highly beneficial for the laboratory to create and maintain a centraltraining file.

Notes:



4.2.1 Comparing Findings Between Audit Team Members



Explanation: The product of the laboratory audit is one checklist that represents a compositeof audit team findings. Auditors are responsible for providing an assessment oflaboratory procedures and their effect on data quality. Assessment of dataquality is straightforward if agreement exists between auditors on QA objectives,QA/QC procedures, and acceptance criteria for these parameters, all of whichshould be clearly identified in the trial burn QAPP. Auditors must discuss andcompare their findings and reach a consensus on positive and negativeobservations for the checklists and on concerns. Reference to the trial burnQAPP, methods, or SOPs may be necessary to resolve differences.

The following questions must be answered:

• Has each measurement of precision and accuracy and eachinstrument calibration that does not meet criteria established inthe method or the trial burn QAPP been discussed in terms of itseffect on sample results?

• Do both auditor checklists agree that an answer is “YES?” Ifso, no further discussion of the specific point is required.

• Do both auditor checklists agree that an answer is “NO?” If so,auditors must resolve whether the issue constitutes a major or aminor concern.

• Do auditor checklists disagree? If so, each auditor must defendhis reasoning, and consensus must be reached.

Check for: “ Have data quality objectives for the trial burn been met?

“ Are auditors in agreement on issues?



Example Situation: Lois notes that, for a given method, laboratory control spikes were not preparedand analyzed at the frequency specified by the trial burn QAPP. The trial burnQAPP specifies that three laboratory control samples should be analyzed, one foreach day of analysis. However, the laboratory performed all of the sampleanalyses first, then analyzed three laboratory control samples sequentially on theday following field sample analysis. Lois identifies this analytical sequence as amajor concern, because the protocol specified in the trial burn QAPP was notfollowed. Clark identifies the same sequence of events, acknowledges that trialburn QAPP protocol was not followed, but considers the effect on data quality tobe minor.

Example Action: Lois and Clark discuss their points of view and consider additional data, such asrecovery of surrogate compounds in samples and recovery of analytes inlaboratory control samples. All surrogate and analyte compound recoveries areacceptable, and Lois and Clark agree that the effect of altering the sequence ofanalyses from trial burn QAPP protocol has had a minimal effect on data qualityand therefore is considered to be a minor concern.

Notes:



4.2.2 Identifying Major Concerns



Explanation: Data quality assessment for a trial burn is straightforward if QA objectives,QA/QC procedures, and acceptance criteria for these parameters are clearlyidentified in the trial burn QAPP. A major concern is any observation applied tothe activity, procedure, method, or documentation being audited that compromisesdata quality.


• Inconsistency with requirements of the risk burn plan for thefacility

• Inadequate QC, based on the U.S. EPA 1990 QA/QC Handbook

• Major modifications of analytical methods cited in the risk burnplan

The following questions must be answered and should have been answered in thecourse of the laboratory audit:

• Has the laboratory followed methods specified in the trial burnQAPP?

• Has the laboratory performed at least the number and type ofQC analyses specified in the trial burn QAPP?

• Has each measurement of precision and accuracy and eachinstrument calibration that does not meet criteria established inthe method or the trial burn QAPP been discussed in terms of itseffect on sample results?

• Has every QC sample been evaluated to ensure that acceptancecriteria presented in the trial burn QAPP have been met?

• Have any issues of data completeness been resolved?

• Do auditors agree on observations of areas of major concern?

Check for: “ Have data quality objectives for the trial burn been met ?




Example Situation: While conducting a laboratory audit, Clark discovers that in the course of loggingwaste feed samples into the laboratory for a series of analyses, a box of sampleswas dropped, and all of the bottles containing waste fuel were broken. The trialburn QAPP specifies that, for waste feed analyses, the laboratory shall make acomposite of a specified number of waste feed samples corresponding to a givensampling run. The laboratory used the remaining bottles of waste fuel to makethe composite and performed the requested analyses using 5 samples rather than10 to make the composite before analysis.

Example Action: The laboratory failed to follow the procedure specified in the trial burn QAPP. Clark considers this failure to be a major concern, because therepresentativeness of the composite waste feed sample was compromised,significantly affecting data quality.

Notes:



4.2.3 Identifying Minor Concerns



Explanation: Minor concerns are deficiencies as applied to the activity, procedure, method, ordocumentation being reviewed, that do not have a significant effect on the qualityof analytical data. Auditors must agree that a specified deficiency does notcompromise the quality of analytical data for the deficiency to be identified as aminor concern.

Some areas of minor concern that might be identified in the laboratory audit are:

• The laboratory has a logbook for preparation of standards thatspecifies the chemical source, the standard preparation date, anda standard expiration date and identifies the preparer of thestandard. However, the label on the standard bottle identifiesonly the preparer and the date of preparation.

• The laboratory has a comprehensive and thorough program fortraining analysts but does not have a central training file.

• The laboratory has SOPs for all methods presently in use in thelaboratory. However, these SOPs are kept only in thelaboratories where they are in use. There is no central file.

• QC samples are checked against trial burn QAPP acceptancecriteria by the analyst and the QA officer. However, thelaboratory does not maintain control charts to monitor QC sampleresults over time.

• Analysts in the laboratory all have notebooks, keep them current,record results, and show all calculations. The notebooks arefrequently checked by the analyst’s peer or supervisor, but thissecondary review is not documented on the page of the notebookbeing checked.

Areas of minor concern in the laboratory usually arise where laboratory practices are adequate to meet trial burn QAPP requirements and, if a questionarises, supporting data are available to answer the question. However, there issome area of deficiency in the completeness of the documentation.

Check for: “ Does the observed deficiency have a significant effect on the quality ofanalytical data?




Example Situation: While conducting a laboratory audit, Lois is informed that in the course of sampleextraction for U.S. EPA Method 0010 train components, a Soxhlet extractor hasgone dry, and the sample cannot be recovered.

Example Action: In this case, the sampling contractor has performed an extra sampling run toprovide a backup sample to be archived, although not required. Because thesample loss occurred within holding times specified for sample extraction, Loisdetermines that substitution of the backup sample for the original sample willhave no significant effect on the quality of the analytical data. Lois considers thelapse in accepted procedures in the laboratory to be a minor concern.

Notes:



4.2.4 Preparing Preliminary Comments



Explanation: Comments to be included in the final audit report generally characterizelaboratory operations, are not considered to be major or minor concerns, and donot require any response on the part of the audited laboratory. Comments by theauditor can be used to describe unusual situations that occurred in the course ofthe laboratory’s analytical activities to support the trial burn and how thelaboratory dealt with the unusual situation. Audit report comments can also beused to acknowledge outstanding performance by the laboratory in some specificarea or to offer suggestions to the laboratory for areas of improvement. Theauditor may also wish to comment on some aspect of the laboratory facility or onspecific analytical procedures or instrumentation.

Material sources to provide comments for the final audit report are the generaland method-specific laboratory checklists, where the auditor may have madecomments in the course of the laboratory walk through. Auditor notes,independent of checklists, may also provide observations on which auditors wishto expand in the final audit report.

Each auditor should collect these comments from checklists and audit notes andcombine them into a preliminary compilation. This preliminary compilation canthen be reviewed by another auditor to ensure that both auditors agree on their observations and wish to comment on the specific area.

Check for: “ Have relevant notes and observations been made by auditors to provideraw material for formulating comments?


Example Situation: In the course of the laboratory audit for the Company XYZ trial burn, Lois andClark note that manufacturers’ requirements for acceptable operating conditionsfor the analytical instrumentation have been met. However, they also note thatwhile acceptable QC practices are in place, the combination of laboratoryhousekeeping practices and crowded facilities results in limited workspace foranalysts and an extremely cluttered laboratory environment.

Example Action: Because the general crowded conditions and poor housekeeping practices at thelaboratory could, at some future time, negatively impact health and safety or dataquality, Lois and Clark encourage the laboratory to improve in these areas orexpand the laboratory into additional space, if available.



Notes:



4.3 PREPARING THE AUDIT REPORT



Explanation: An audit report is prepared as a result of a laboratory audit. The audit reportrepresents a consensus of the auditing team and includes a textual audit reportand a composite for each of the checklists prepared by individual auditors.

Check for: The textual audit report incorporates the following sections:

“ Overview of the trial burn test (Section 4.3.1)

“ Overview of the laboratory (Section 4.3.2)

“ Summary of auditor concerns (Section 4.3.3)

“ Summary of comments (Section 4.3.4)

“ Recommendations (Section 4.3.5)

“ Conclusions (Section 4.3.6)

The following sections describe each part of the audit report.

Example Situation: Lois and Clark prepare the report and use discussions of complex analyticalmechanisms; however, the ultimate reader and user of the report is a nonchemist. The reader is confused and frustrated by the report.

Example Action: While the findings of the audit may deal with complex chemistries, the readersimply needs to know if the findings reflect a potential for invalid data. Theauditor should consider the reader’s background and ultimate purpose of thereport before beginning to write. Lois and Clark revise the report to explain theirfindings in a clearer, less technical manner.

Notes:



4.3.1 Overview of the Trial Burn Test



Explanation: The section of the audit report discussing the TBP overview should include thefollowing information:

• Brief summary of the unit being tested, the trial burn test design,the sampling and analytical methods being used, and the goal ofthe test. Adequate information to provide the level of detaildesired for this section will be available in the facility TBP andtrial burn QAPP

C Description of why the laboratory audits are being conducted

• Description of the laboratory or laboratories being audited,including laboratory name and address, key contacts, analyses,and matrices analyzed

• Summary of audit activities at each audited laboratory

Check for: “ Has complete information regarding laboratory location, key contacts,matrices analyzed, and analyses performed been obtained for eachlaboratory?

“ Is sufficient information available in the trial burn QAPP to provide adescription of the facility where the trial burn is occurring?

“ Have auditors been careful to verify the correct spelling of names,accuracy of addresses, and other information that will be used in theaudit report?

“ Have auditors been careful to verify that the laboratory name is completeand correct?

Example Situation: The sign on the outside of the laboratory building when Lois and Clark arrivesays “Smith.” Upon exchange of business cards, auditors find that the companyis named “Smith Laboratories.” On the corporate brochure, the organization isdescribed as “Smith Environmental Laboratories, Inc.”

Example Action: During the audit, Lois asks the company president to verify the correct name ofhis company for the audit report.



Notes:

4.3.2 Overview of the Laboratory



Explanation: The section of the audit report discussing the laboratory overview should includethe following information:

• Brief discussion of the analyses the laboratory is conducting forthis trial burn

• Description of laboratory functions (which analyses does thelaboratory perform, not limited to analyses specifically for thetrial burn). Company brochures, which can be requested by theauditors either prior to the laboratory audit or at the time of theaudit, are usually very useful for providing information aboutlaboratory capabilities.

• Brief description of physical facilities of the laboratory. Company brochures, which can be requested by the auditorseither prior to the laboratory audit or at the time of the audit, areusually very useful for providing information about laboratoryfacilities.

• Brief discussion of the laboratory organization, including keypersonnel and their responsibilities. Auditors shouldacknowledge specifically the laboratory staff member withoverall responsibility for guiding the laboratory walkthrough andlocating requested information.

Check for: “ Has complete information regarding laboratory location, key contacts,matrices analyzed, and analyses performed been obtained for eachlaboratory?

“ Have auditors collected information to be able to provide a short description of laboratory physical facilities?

“ Have auditors been careful to verify the correct spelling of names andaccuracy of addresses and other information that will be used in the auditreport?



“ Have auditors been careful to verify the names of key personnel andtheir functions in the laboratory?

Example Situation: Lois and Clark disagree as to the level of detail to include in the laboratoryoverview with regard to the actual square footage of the radiochemistrylaboratory; however, no radiochemistry analyses were required for the project.

Example Action: The information included should have relevance to the performance of analyticalservices for the project. The square footage of a laboratory is valuableinformation, especially when the facility is very small, because the potential forbumping into equipment and dropping samples and extracts is high. However, ifthe particular laboratory area is not being utilized for the project, the concernbecomes negligible and should not be included in the report. After furtherdiscussion, Lois and Clark decide not to include the square footage of that portionof the laboratory in the laboratory overview.

Notes:



4.3.3 Summarizing Concerns



Explanation: The section of the audit report discussing concerns should be divided into majorand minor concerns. The following deficiencies, if present as applied to theactivity, procedure, method, or documentation being reviewed, would beconsidered major:

• Inconsistency with requirements of the project-specific approvedQAPP

• Insufficient QC, based on U.S. EPA’s “Handbook: QA/QCProcedures for Hazardous Waste Incineration” (U.S. EPA1990)

• Major unauthorized modifications of analytical methods cited inthe project-specific approved QAPP

Major concerns have a significant impact on the quality of the data beinggenerated. Minor concerns are deficiencies that apply to the activity, procedure,method or documentation being reviewed that do not have a significant impact onthe quality of the data being generated.

For example, items such as laboratory substitution of an alternative analyticalmethod for the analytical method specified in the trial burn QAPP or failure toanalyze samples within hold times specified by the method would be majorconcerns. Items such as a lack of documentation of laboratory training recordsor calculating analytical results in the wrong units would be minor concerns.

The audit report should address:

“ Definition of what constitutes a major concern

“ Listing of any major concerns as determined by auditor consensus

“ Explanation and discussion of each major concern, including the auditor’sobservation and any discussion with laboratory staff involving the majorconcern

“ Definition of what constitutes a minor concern

“ Listing of any minor concerns as determined by auditor consensus



“ Explanation and discussion of each minor concern, including the auditor’sobservation and any discussion with laboratory staff involving the majorconcern

Example Situation: Not applicable to this section of the manual.

Example Action: Not applicable to this section of the manual.

Notes:



4.3.4 Summarizing Comments



Explanation: The section of the audit report discussing comments should include the followinginformation:

• Definition of a comment, pointing out that comments are notconsidered to be major or minor concerns and do not require anyresponse on the part of the laboratory

• Concise discussion of each comment on which the auditing teamagrees

• Concise discussion of laboratory procedures

Check for: “ Auditors must reach consensus on comments. No comment should beincluded in the audit report unless auditors agree on its relevance.

Example Situation: Lois and Clark are very impressed with the personalities, generosity, hospitality,and visual aesthetics of the laboratory personnel and facility. It is common towant to include positive comments regarding these items in the report; however,often such comments are published in sales brochures and other propaganda thatthe laboratory produces for marketing purposes.

Example Action: Lois and Clark refrain from making complimentary remarks about the laboratoryin the audit report, because comments of this nature do not directly affect theintegrity of sample data.

Notes:



4.3.5 Preparing Recommendations



Explanation: This section of the audit report can include other observations that would improvedata from the audited laboratory. Recommendations require no action and do notaffect the results of a particular audit. However, recommendations could includethe following information:

• Suggestions by auditors for improvements in laboratoryoperations

• Suggestions by auditors for improvements in laboratorydocumentation

• Suggestions by auditors for improvements in laboratorycommunication

• Suggestions that auditors feel will improve the quality of thelaboratory’s analytical data

Check for: “ Auditors must reach consensus on recommendations. Norecommendation should be included in the audit report unless auditorsagree on its relevance.

Example Situation: Lois and Clark observe that the laboratory’s reporting section does not havesufficient space to archive all data in an accessible way and are inclined toprovide detailed solutions to the data archival problem.

Example Action: Auditors should refrain from providing or requiring a specific solution toproblems. In this report, Lois and Clark suggest that the archival problem ofinsufficient space be solved, because data archival is important to the projectbeing reviewed. The laboratory should be allowed to explore possibilities andreport a solution by a given date.

Notes:



4.3.6 Preparing the Conclusions



Explanation: The section of the audit report discussing conclusions should include the followinginformation:

• Conclusions by auditors that data quality objectives for the trialburn have or have not been met because of laboratory operations

• Assessment of whether any of the laboratory operations have anadverse effect on data quality

• General conclusions regarding laboratory competence and staff

Check for: “ Auditors must reach consensus on conclusions. No conclusion should beincluded in the audit report unless auditors agree on its relevance.

Example Situation: Lois and Clark find that the ICP’s precision is not as good as its potential and thatdetection limits are unusually high for several metals. Lois and Clark want toinclude the issue in the major comment section and conclude that the instrumentis incapable of operating to its potential. However, in reviewing the trial burnQAPP, they note that the high detection limits are sufficient to meet thesensitivity objective of the trial burn.

Example Action: Lois and Clark decide to place the comment about the ICP’s detection limits inthe comment section only and not present it as a major or minor concern,because the overall trial burn objectives have been met.

Notes:

ATTACHMENT A

LABORATORY AUDIT CHECKLIST

(14 Sheets)

Laboratory Name: Reviewers: Date Completed:

5-A-1

SECTION I GENERAL INFORMATION

Reviewers: Date Completed:

Facility Representative:

Facility Name: Address of Facility:

Telephone No.:

Evaluation Firm:

Names of inspectors: Date(s) of inspection:

I - 1 SECTION II QUALITY ASSURANCE MANUAL


5-A-2

Requirements Yes No NA Comments (Explain all negative responses)

Determine if the laboratory’s quality assurance manual includes the following:

Names an individual as the laboratory quality assurance manager and specifiesjob requirements for the position?

Includes a current summary of training, experience, and job description requiredfor each member of the laboratory staff?

Describes quality control paperwork flow and identifies those who areauthorized to approve data and results?

Identifies personnel responsible for corrective action procedures?

Describes the laboratory's system for developing or revising technical proceduresand identifies those who have authorization to do so?

Requires dating chemicals upon receipt and using them on a first-in, first-outbasis?

Specifies use of reagent-grade or high-purity chemicals to prepare standards?

Requires testing of chemicals used in analyses to ensure they contain nocontaminants that may interfere with analyses?

Requires labeling of all reagents and solutions to indicate identity, concentration, storage requirements, preparer's name, preparation date, and expiration date?

Requires routine checking and recording of the conductivity of distilled anddemineralized water?

II - 1



5-A-3

Specifies use of reagent-grade water, as required by the specific method?

Specifies use of distilled water, as required by the specific method?

Requires discontinuing the use of any reagents or solutions labeled withexpiration dates that have passed?

Requires storage of samples and standards containing analytes of interest in areasother than those where trace analysis is performed?

Requires storage of standards separately from sample extracts?

Specifies the use of analysis request sheets or work orders?

Includes and requires the use of written calibration procedures, analyticalprocedures, computational procedures, quality control procedures, and operatingprocedures?

Specifies the use of standard curves and check samples for calibration purposes?

Specifies the use of logs to record all instrument and equipment checks?

Describes when an analytical system is "out of control" through internal qualitycontrol samples?

Requires corrective procedures when an analytical system is "out of control"?

Specifies the use of Class A glassware?

Names a sample custodian in the laboratory?

II - 2



5-A-4

Describes storage requirements for incoming samples?

Specifies the assignment of unique laboratory numbers to all incoming samples?

Requires maintenance of proper temperatures for incoming samples?

Describes chain-of-custody procedures that the laboratory will use?

Specifies the use of a master schedule sheet or logbook of all samples being analyzed, indexed by laboratory numbers, client, date of arrival, and analysis tobe performed?

Specifies maximum holding times for samples?

Requires the daily temperature recordings in cold storage areas?

Specifies the use of matrix spikes (one per analytical batch per matrix, or one perevery 20 samples, whichever is more frequent)?

Requires the use of laboratory duplicates (one per analytical batch per matrix, orone per every 20 samples, whichever is more frequent)?

Requires the use of blanks (one per analytical batch per matrix, or one per every20 samples, whichever is more frequent)?

Requires the use of field duplicates (one per analytical batch, or one per every 20samples, whichever is more frequent)?

Requires the use of check samples (one per analytical batch, or one per every 20samples, whichever is more frequent)?

Requires the use of surrogates for volatile and semivolatile organics and pesticides(added to every blank, standard, sample, and quality control sample)?

II - 3



5-A-5

Requires gas chromatograph/mass spectrometer (GC/MS) instrumentperformance check (in which the initial five-point calibration is verified with asingle-point calibration once every 12 hours of instrument operation and, if thesensitivity and linearity criteria are not met, a new five-point initial calibrationmust be generated)?

Requires a system that independently examines and validates raw data from thelaboratory?

Requires owner/operator to have a system that examines and validates raw datawhen a subcontractor laboratory is used?

II - 4


5-A-6


5-A-7

SECTION III PERSONNEL


Review the laboratory's personnel qualifications and organizational structure.

Has the laboratory appointed a quality assurance manager who routinelyperforms the following actions:

- Ensures adherence to quality assurance requirements for sampling?

- Ensures that all test and measuring equipment are properly calibrated?

- Monitors logging in of samples?

- Approves project plans, specific analyses, and final reports?

- Maintains a copy of the master schedule sheet?

- Maintains separate copies of all methods performed by the laboratory?

- Maintains written and signed records of periodic inspections?

- Maintains all quality assurance records in one location?

Are qualified individuals used to perform the required analyses?

Does the laboratory have a documented program of personnel training?

Does the laboratory routinely verify proficiency of personnel in the variousmethods?

Are qualified individuals authorized to approve data and results?

III - 1


5-A-8

SECTION IV GENERAL LABORATORY SUPPLIES AND EQUIPMENT


Review the procedures for maintaining the laboratory's supplies and equipment.

Are adequate laboratory facilities and instruments available to perform therequired analyses?

Is the solvent storage area properly vented and appropriate for the preventionof possible laboratory contamination?

Are analytical and sample storage areas isolated from all atmospheric sources ofsolvent?

Are chemicals dated upon receipt and used on a first-in, first-out basis?

Are reagent-grade or high-purity chemicals used to prepare standards?

Are chemicals used in analyses tested to ensure that they contain nocontaminants that may interfere with the analyses?

Are all reagents and solutions labeled to indicate identity, concentration, storagerequirements, preparer's name, preparation date, and expiration date?

Is a source of distilled or demineralized water available?

Is the conductivity of distilled or demineralized water routinely checked andrecorded?

Is reagent-grade water used for organic methods?

Is distilled water used for inorganic methods?

Are any of the reagents or solutions being used labeled with an expiration datethat has passed?

To avoid contamination, are samples and standards containing the analytes ofinterest stored or used in areas other than those where trace analysis isperformed?



5-A-9

IV - 1



5-A-10

Are standards stored separately from sample extracts?

Do chemical handling areas consist of either a stainless-steel bench or animpervious material covered with absorbent materials?

Are contamination-free areas provided for trace level or organic analytical work?

Are exhaust hoods provided to allow contamination-free work with volatilematerials (that is, venting for preparation, extraction, and analysis)?

Is an adequate supply of routinely needed in-house replacement parts availableto ensure that analytical equipment is not inoperable during a critical period?

Is a service record logbook maintained for each analytical instrument?

Are instruments properly vented and appropriate traps in place, as required?

Are chemical waste disposal policies and procedures well-defined and followedby the laboratory?

Is Class A glassware used or is it calibrated to ensure that the amount markedon the glassware coincides with the amount delivered?

Is the glassware cleaned correctly after each use to ensure that there will be nocontamination with the next use?

Is the analytical balance located away from drafty areas and areas subject torapid temperature changes?

Has a certified technician calibrated and checked the balance within 1 year?

IV - 2


5-A-11


5-A-12

SECTION V SAMPLE RECEIPT AND STORAGE


Review sample handling procedures at the laboratory.

Is a sample custodian appointed to log incoming samples?

Is a written SOP available that describes sampling requirements (such as, type ofsampling container, preservation technique, and storage container) for eachanalysis?

If no custodian is appointed, are the individuals logging in samples aware of thesampling requirements for each analysis?

Does the custodian know the process for storing incoming samples?

Is a sample label affixed to each container?

Do sample labels contain information sufficient to identify the sample and ensurethat it is has been sampled in the correct manner (including facility name, stationnumber, date sampled, time sampled, type of analysis requested, preservationused, and signature of sampler)?

Are samples collected in the type of container specified for each analysis?

Are samples preserved as required and cooled to 4EC?

Do samples shipped to the laboratory arrive at the correct temperature to ensurethat the sample has remained in a preserved state?

Are water samples for volatile analyses checked for air bubbles?

Are trip blanks, field blanks, and field duplicates used as required?

If so, are they identified as such?



5-A-13

V - 1



5-A-14

If used, are spiked samples identified?

Is a chain-of-custody form filled out and kept on file?

Is the information on the sample tag and chain-of-custody form verified andmatched?

Are unique laboratory numbers assigned to all incoming samples (including qualitycontrol samples)?

Does the laboratory maintain a master schedule sheet or logbook of all samplesbeing analyzed, indexed by laboratory number, client, date of arrival, and analysisto be performed?

Is the laboratory number written on the sample label, the master schedule sheet,and any documents related to that sample?

Are completed sample analysis work orders available for each sample?

Does each sample have a separate work order for each analysis or group ofanalyses (that is, organic and inorganic) to be performed (to ensure that eachanalyst who must perform an analysis on that sample will have a work order)?

After all analyses have been completed, are all work orders attached to allappropriate summary sheets for each analysis?

Are all samples analyzed within required holding times?

Are samples maintained at the correct temperature until the time of analysis?

Are adequate facilities provided for storage of incoming samples, including coldstorage?

Are volatile samples stored separately from nonvolatile or semivolatile samples?

Is the temperature of the cold storage recorded daily in a logbook?

V - 2



5-A-15

Are temperatures outside of control limits noted, and are appropriate actionstaken when required?

If reused, are sample containers cleaned properly?

Are the possession and handling of samples traceable from the time and date ofcollection to the time and date of analysis and reporting?

Demonstrate by tracing at least one sample in the laboratory. Summarize bycompleting Form V-1.



5-A-16

V - 3


5-A-17

FIGURE V-1Sample Tracing Form

Use this form to demonstrate the traceability of samples from collection to reporting.

Trace at least one sample from the trial burn facility through the laboratory systems.

Sample ID Information Sample A Sample B Sample C Comments (Explain all negative responses)

Field Sample Number

Laboratory Name

Laboratory Address

Sample Collection Location

Sampler Name or Initials

Date Sampled

Time Sampled

Date Received at Laboratory

Laboratory Sample Number

Analyses Requested

Storage Procedures

Date of Sample Preparation

Date of Sample Analysis

Analysts’ Initials

Methods Used

Date Results Reported

V - 4


5-A-18

SECTION VI QUALITY CONTROL PROGRAM


Does the laboratory appear to have sufficient capacity to prepare and analyze allsamples within holding times?

Is one matrix spike used for every analytical batch or every 20 samples, whichever is most frequent?

Are matrix spike accuracies analyzed to establish that the analytical measurementsystem is functioning properly with the desired sensitivity?

Are precision results of sample replicates measured for each method to indicatereproducibility among individual measurements of the same property undersimilar conditions?

Are the precision and accuracy results used to determine the control limits for alloperating parameters?

Are these precision and accuracy results organized in the form of quality controlcharts?

Are quality control charts or tabulation of mean and standard deviation (or theequivalent) used to document the validity of data on an as-run basis?

Are matrix spike results compared to control charts on an as-run basis todetermine whether the analysis is "in control"?

Is one check sample used per analytical batch or every 20 samples, whichever ismore frequent?

Is one laboratory method blank used per analytical batch or every 20 samples,whichever is more frequent, to ensure that there are no contaminants that mayinterfere with the analysis?

Is one field duplicate used per analytical batch or every 20 samples, whichever ismore frequent?

Are laboratory duplicates prepared and analyzed per analytical batch or every 20samples, whichever is more frequent (not including reinjection or reanalysis ofsame set of standards or samples)?



5-A-19

VI - 1SECTION VII DATA HANDLING AND REPORTING


Review procedures for data handling, reporting, and recordkeeping.

Are computerized and manual checks applied at various appropriate levels of themeasurement process to ensure data validation?

Are the data validation criteria documented (including limits on operationalparameters, calibration data, special checks, statistical tests, and manual checks)?

Does the laboratory have procedures for data handling and reporting, includingthe recording of data on standard forms and in laboratory notebooks?

If so, is this reporting format described with example forms provided?

Are sample calculations available for inspection?

Are bound notebooks used for all laboratory activities?

Do notebooks, logbooks, and run logs have the following pertinent data:

- Title - describing the activity being recorded- Instrumentation - type and ID number (for example GC #3)- Date of preparation or analysis- Initials of preparer or analyst- For preparation notebooks or logbooks - details of activity, such as sample

measurements, reagents and quantities, and procedure times, if applicable- For instruments runlogs - run sequences, identity of each sample and analyte- Units of measurements- Calculations, if applicable- Peer or supervisory review signature and date

Are notebooks reviewed by a peer or supervisor (as indicated by a signature anddate)?

Are raw data archived and documented properly?

Are records readily available for review?


5-A-20

Are records maintained for at least 3 years?

VI - 2

Documents

Hazardous Waste Combustion Unit · American Society for Testing and Materials (ASTM). “Annual Book of ASTM Standards.” Philadelphia, Pennsylvania. Annual Series. U.S. Environmental